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Sample records for immunoaffinity chromatography iac

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

    Science.gov (United States)

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

  2. Purification of antibody against Ara h 2 by a homemade immunoaffinity chromatography column.

    Science.gov (United States)

    Wu, Zhihua; Li, Kun; Zhan, Shaode; Tong, Ping; Li, Xin; Yang, Anshu; Chen, Hongbing

    2017-09-14

    Antibodies are used extensively in numerous applications both in vivo and in vitro. To purify anti-Ara h 2 polyclonal antibody, a homemade immunoaffinity chromatography (IAC) column method was established. The properties of homemade column were compared with those of the mAb affinity protein G (MPG) agarose high flow, a commercially available column successfully used in capturing polyclonal antibodies. During antibody purification from rabbits' antiserum against Ara h 2, the column capacity, recovery, and purification factor were characterized for IAC and MPG. The homemade IAC could separate the corresponding antibody with higher specificity and lower cost but with lower recovery and column capacity than those of MPG. Thus, the homemade IAC is a specific, inexpensive, and suitable method that can be used for various laboratory purifications.

  3. Calcium-sensitive immunoaffinity chromatography

    DEFF Research Database (Denmark)

    Henriksen, Maiken L; Lindhardt Madsen, Kirstine; Skjoedt, Karsten

    2014-01-01

    Immunoaffinity chromatography is a powerful fractionation technique that has become indispensable for protein purification and characterization. However, it is difficult to retrieve bound proteins without using harsh or denaturing elution conditions, and the purification of scarce antigens...... to homogeneity may be impossible due to contamination with abundant antigens. In this study, we purified the scarce, complement-associated plasma protein complex, collectin LK (CL-LK, complex of collectin liver 1 and kidney 1), by immunoaffinity chromatography using a calcium-sensitive anti-collectin-kidney-1 m...... chromatography was superior to the traditional immunoaffinity chromatographies and resulted in a nine-fold improvement of the purification factor. The technique is applicable for the purification of proteins in complex mixtures by single-step fractionation without the denaturation of eluted antigens...

  4. Polyglycidyl methacrylate based immunoaffinity cryogels for insulin adsorption

    International Nuclear Information System (INIS)

    Memmedova, Türkan; Armutcu, Canan; Uzun, Lokman; Denizli, Adil

    2015-01-01

    Immunoaffinity chromatography (IAC) is a kind of bioaffinity chromatography which used antibodies or antibody-related molecules as the stationary phase. IAC is used by many applications for analytical, clinical and diagnostic purposes, particularly preferring in analytical purposes on one-step separation and purification of target compounds. Moreover, immunoaffinity chromatography is used in antibody enrichment and separation of cells. IAC columns are usually applied in the antibody experiments due to powerful and selective binding of antibodies and/or their target antigens. Antigen or antibody molecules could be immobilized to the solid support. Therefore, target antibody or cell is purified. Specific bioligands can be immobilized directly on glycidyl based polymeric material with simple acid–base catalyst. In this study, polyglycidyl methacrylate based therefore cryogels were prepared and anti-insulin antibodies were immobilized on porous surface of cryogels. Swelling test, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM) were conducted to characterize cryogels developed. To optimize separation conditions, effects of pH, initial insulin concentration, flow rate, salt concentration, contact time and temperature on insulin adsorption capacity were examined. The results indicated that the immunoaffinity cryogel developed here could be classified as good alternative with prominent properties such as high reusability and cost-friendly adsorbent and would be one of the primary reports for immunoaffinity purification of insulin molecules in not only lab-scale but also for industrial purposes. - Highlights: • Polyglycidyl methacrylate based cryogels developed as stationary phase • Immunoaffinity cryogels for reusable and cost-friendly insulin adsorption • Increase in worldwide prevalence of diabetes, type 1 or 2 • An exponential increase in the demand on insulin market • Guiding researchers for not

  5. Polyglycidyl methacrylate based immunoaffinity cryogels for insulin adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Memmedova, Türkan; Armutcu, Canan; Uzun, Lokman, E-mail: lokman@hacettepe.edu.tr; Denizli, Adil

    2015-07-01

    Immunoaffinity chromatography (IAC) is a kind of bioaffinity chromatography which used antibodies or antibody-related molecules as the stationary phase. IAC is used by many applications for analytical, clinical and diagnostic purposes, particularly preferring in analytical purposes on one-step separation and purification of target compounds. Moreover, immunoaffinity chromatography is used in antibody enrichment and separation of cells. IAC columns are usually applied in the antibody experiments due to powerful and selective binding of antibodies and/or their target antigens. Antigen or antibody molecules could be immobilized to the solid support. Therefore, target antibody or cell is purified. Specific bioligands can be immobilized directly on glycidyl based polymeric material with simple acid–base catalyst. In this study, polyglycidyl methacrylate based therefore cryogels were prepared and anti-insulin antibodies were immobilized on porous surface of cryogels. Swelling test, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, and scanning electron microscopy (SEM) were conducted to characterize cryogels developed. To optimize separation conditions, effects of pH, initial insulin concentration, flow rate, salt concentration, contact time and temperature on insulin adsorption capacity were examined. The results indicated that the immunoaffinity cryogel developed here could be classified as good alternative with prominent properties such as high reusability and cost-friendly adsorbent and would be one of the primary reports for immunoaffinity purification of insulin molecules in not only lab-scale but also for industrial purposes. - Highlights: • Polyglycidyl methacrylate based cryogels developed as stationary phase • Immunoaffinity cryogels for reusable and cost-friendly insulin adsorption • Increase in worldwide prevalence of diabetes, type 1 or 2 • An exponential increase in the demand on insulin market • Guiding researchers for not

  6. On-line immunoaffinity column-liquid chromatography-tandem mass spectrometry method for trace analysis of diuron in wastewater treatment plant effluent sample.

    Science.gov (United States)

    Zhang, Xiuli; Martens, Dieter; Krämer, Petra M; Kettrup, Antonius A; Liang, Xinmiao

    2006-11-10

    An on-line immunoaffinity column with liquid chromatography/tandem mass spectrometry (IAC-LC-MS/MS) method for the determination of diuron in water matrices was described. This method used a sol-gel immunoaffinity column (20 mm x 4 mm I.D.) for on-line sample cleanup and enrichment, a monolithic analytical column (100 mm x 4.6 mm I.D.) for separation, and a triple quadrupole mass spectrometer for quantitation. The major challenges for the on-line set-up were discussed. The optimized on-line protocol was emphasized by the fact that low limit of quantitation (LOQ) of 1.0 ng/L was achieved with only 2.5-mL sample. In addition, a satisfactory accuracy ( approximately 90% of recovery) and precision (effect, the on-line IAC-LC-MS/MS analysis method can reliably determine diuron in wastewater treatment plant effluent sample.

  7. Determination of zearalenone content in cereals and feedstuffs by immunoaffinity column coupled with liquid chromatography.

    Science.gov (United States)

    Fazekas, B; Tar, A

    2001-01-01

    The zearalenone content of maize, wheat, barley, swine feed, and poultry feed samples was determined by immunoaffinity column cleanup followed by liquid chromatography (IAC-LC). Samples were extracted in methanol-water (8 + 2, v/v) solution. The filtered extract was diluted with distilled water and applied to immunoaffinity columns. Zearalenone was eluted with methanol, dried by evaporation, and dissolved in acetonitrile-water (3 + 7, v/v). Zearalenone was separated by isocratic elution of acetonitrile-water (50 + 50, v/v) on reversed-phase C18 column. The quantitative analysis was performed by fluorescence detector and confirmation was based on the UV spectrum obtained by a diode array detector. The mean recovery rate of zearalenone was 82-97% (RSD, 1.4-4.1%) on the original (single-use) immunoaffinity columns. The limit of detection of zearalenone by fluorescence was 10 ng/g at a signal-to-noise ratio of 10:1 and 30 ng/g by spectral confirmation in UV. A good correlation was found (R2 = 0.89) between the results obtained by IAC-LC and by the official AOAC-LC method. The specificity of the method was increased by using fluorescence detection in parallel with UV detection. This method was applicable to the determination of zearalenone content in cereals and other kinds of feedstuffs. Reusability of immunoaffinity columns was examined by washing with water after sample elution and allowing columns to stand for 24 h at room temperature. The zearalenone recovery rate of the regenerated columns varied between 79 and 95% (RSD, 3.2-6.3%). Columns can be regenerated at least 3 times without altering their performance and without affecting the results of repeated determinations.

  8. Off-line coupling of multidimensional immunoaffinity chromatography and ion mobility spectrometry: A promising partnership.

    Science.gov (United States)

    Armenta, Sergio; de la Guardia, Miguel; Abad-Fuentes, Antonio; Abad-Somovilla, Antonio; Esteve-Turrillas, Francesc A

    2015-12-24

    The extreme specificity of immunoaffinity chromatography (IAC) columns coupled to the high sensitivity of ion mobility spectrometry (IMS) measurements makes this combination really useful for rapid, selective, and sensitive determination of a high variety of analytes in different samples. The capabilities of the IAC-IMS coupling have been highlighted under three different scenarios: (i) multiclass residue analysis using a single IAC column, (ii) multiclass residue analysis using stacked IAC columns, and (iii) isomer analysis. In the first case, the determination of three strobilurin fungicides - azoxystrobin, picoxystrobin, and pyraclostrobin - in water and strawberry juice was considered, obtaining limits of quantification (LOQs) from 11 to 63μgL(-1). Recoveries from 96 to 106% for water, and from 67 to 104% for strawberry juice were obtained. In the second case, anilinopyrimidine compounds, including two analytes with similar drift time, were selectively retained in different IAC columns and analyzed after independent elution in commercial wine samples by IMS. LOQ values of 16, 14 and 12μgL(-1) were obtained for pyrimethanil, mepanipyrim, and cyprodinil, respectively. The obtained recoveries for wine samples spiked with 25 and 100μgL(-1) were from 82 to 123%. Additionally, the stacked IAC columns concept was applied to the separation of Z and E isomers of azoxystrobin that were selectively retained in specific IAC columns and quantified by IMS. Recoveries between 91 and 94% were obtained for both isomers in water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Immunoaffinity chromatography of abscisic acid combined with electrospray liquid chromatography–mass spectrometry

    Czech Academy of Sciences Publication Activity Database

    Hradecká, Veronika; Novák, Ondřej; Havlíček, Libor; Strnad, Miroslav

    2007-01-01

    Roč. 847, č. 2 (2007), s. 162-173 ISSN 1570-0232 R&D Projects: GA MŠk(CZ) LC06034; GA AV ČR IBS5038351 Institutional research plan: CEZ:AV0Z50380511 Source of funding: V - iné verejné zdroje ; V - iné verejné zdroje Keywords : abscisic acid * immunoaffinity chromatography * liquid chromatography-mass spectrometry Subject RIV: ED - Physiology Impact factor: 2.935, year: 2007

  10. Enantiomeric quantification of (S)-(+)-methamphetamine in urine by an immunoaffinity column and liquid chromatography-electrospray-mass spectrometry

    International Nuclear Information System (INIS)

    Lua, Ahai C.; Sutono, Yenny; Chou, T.-Y.

    2006-01-01

    A method using an immunoaffinity column (IAC) and liquid chromatography-electrospray ionization mass spectrometry (LC/MS) for on-line detecting the presence of MA in the effluent was developed for the quantitative and enantiomeric determination of (S)-(+)-methamphetamine (D-MA) in urine. The IAC was made in our laboratory and utilized in the LC/MS to simultaneously extract and separate enantiomers of MA from urine samples. An aqueous ammonium acetate buffer was used as the mobile phase. Urine samples were spiked with racemic deuterated methamphetamine (MA-d 14 ) as internal standard (IS), filtered through a membrane, and injected into the LC/MS without any further pre-treatment. Protonated molecular ion of MA and MA-d 14 (m/z 150 and 164) were isolated and further fragmented, the respective product ions, m/z 119 and 130, were collected for quantitative determination. This is an improvement of our previous method (A.C. Lua, Tsong-Yung Chou, J. Chromatogr. A 967 (2002) 191). In the previous method, MA was separated with HPLC, the efflux was fractionated and each fraction was either determined with an immunoassay or GC/MS. Monitoring of MA in the efflux is tedious and time consuming. Urine samples spiked with different concentrations of D-MA were measured by this method. A linear relationship exists in the 150-1050 ng/mL range, and the detection limit (defined as signal-to-noise ratio 3) of D-MA was determined to be 18 ng/mL. The linearity of the method for D-MA can be described by the equation (Y = 1.415 x 10 -3 X + 0.034, correlation coefficient: r 2 = 0.999). Within run, accuracy and precision (n = 6, relative error: -7.2 to +4.0% and relative standard deviation: 3.8-9.3%) of the method are fairly good

  11. Enantiomeric quantification of (S)-(+)-methamphetamine in urine by an immunoaffinity column and liquid chromatography-electrospray-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Lua, Ahai C. [Department of Laboratory Medicine and Biotechnology and Graduate Institute of Medical Biotechnology, Tzu Chi University, 701, Chung Yang Road Section 3, Hualien, 970, Taiwan (China); Sutono, Yenny [Department of Laboratory Medicine and Biotechnology and Graduate Institute of Medical Biotechnology, Tzu Chi University, 701, Chung Yang Road Section 3, Hualien, 970, Taiwan (China); Chou, T.-Y. [Department of Laboratory Medicine and Biotechnology and Graduate Institute of Medical Biotechnology, Tzu Chi University, 701, Chung Yang Road Section 3, Hualien, 970, Taiwan (China)]. E-mail: cty@mail.tcu.edu.tw

    2006-08-18

    A method using an immunoaffinity column (IAC) and liquid chromatography-electrospray ionization mass spectrometry (LC/MS) for on-line detecting the presence of MA in the effluent was developed for the quantitative and enantiomeric determination of (S)-(+)-methamphetamine (D-MA) in urine. The IAC was made in our laboratory and utilized in the LC/MS to simultaneously extract and separate enantiomers of MA from urine samples. An aqueous ammonium acetate buffer was used as the mobile phase. Urine samples were spiked with racemic deuterated methamphetamine (MA-d{sub 14}) as internal standard (IS), filtered through a membrane, and injected into the LC/MS without any further pre-treatment. Protonated molecular ion of MA and MA-d{sub 14} (m/z 150 and 164) were isolated and further fragmented, the respective product ions, m/z 119 and 130, were collected for quantitative determination. This is an improvement of our previous method (A.C. Lua, Tsong-Yung Chou, J. Chromatogr. A 967 (2002) 191). In the previous method, MA was separated with HPLC, the efflux was fractionated and each fraction was either determined with an immunoassay or GC/MS. Monitoring of MA in the efflux is tedious and time consuming. Urine samples spiked with different concentrations of D-MA were measured by this method. A linear relationship exists in the 150-1050 ng/mL range, and the detection limit (defined as signal-to-noise ratio 3) of D-MA was determined to be 18 ng/mL. The linearity of the method for D-MA can be described by the equation (Y = 1.415 x 10{sup -3} X + 0.034, correlation coefficient: r {sup 2} = 0.999). Within run, accuracy and precision (n = 6, relative error: -7.2 to +4.0% and relative standard deviation: 3.8-9.3%) of the method are fairly good.

  12. Immunoaffinity chromatography for the sample pretreatment of Taxus plant and cell extracts prior to analysis of taxanes by high-performance liquid chromatography

    NARCIS (Netherlands)

    Theodoridis, G; Haasnoot, W; Schilt, R; Jaziri, M; Diallo, B; Papadoyannis, IN; de Jong, GJ; Cazemier, G.

    2002-01-01

    The application of immunoaffinity chromatography for the purification of Taxus plant and cell extracts prior to the HPLC analysis is described. Polyclonal antibodies raised against 10-deacetylbaccatin III (10-DAB III), paclitaxel's main precursor in plant, were characterised by enzymed-linked

  13. Liquid chromatography-high resolution mass spectrometry with immunoaffinity clean-up for the determination of the oxidative stress biomarker 8-iso-prostaglandin F2alpha in wastewater.

    Science.gov (United States)

    Ryu, Yeonsuk; Reid, Malcolm J; Thomas, Kevin V

    2015-08-28

    A reliable oxidative stress biomarker, 8-iso-prostaglandin F2α (8-iso-PGF2α), was for the first time quantitatively analysed in wastewater using an analytical method consisting of liquid chromatography-high resolution mass spectrometry coupled to immunoaffinity clean-up (IAC-LC-HRMS). Factors influencing the method's robustness were investigated, including analyte stability in sewage and enzymatic deconjugation with β-glucuronidase. The IAC-LC-HRMS method was linear over the range of 0.1-100ng/mL with correlation coefficient (R(2)) of 0.999. The quantification limits were sufficiently low to detect 8-iso-PGF2α in sewage (method quantification limit of 0.3ng/L) and precision, expressed as relative standard deviation was less than 7% and the accuracy expressed as relative recovery was in the 103-113% range. As a result, the application of the method to 24-h composite wastewater samples from Oslo showed 8-iso-PGF2α concentrations of 18.9-23.3ng/L for 8 days in March 2015. This study demonstrates a standard method to analyse 8-iso-PGF2α in sewage that will contribute to the further investigation of the potential use of 8-iso-PGF2α as a sewage biomarker for assessing the status of community health. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Simultaneous identification and quantification of tetrodotoxin in fresh pufferfish and pufferfish-based products using immunoaffinity columns and liquid chromatography/quadrupole-linear ion trap mass spectrometry

    Science.gov (United States)

    Guo, Mengmeng; Wu, Haiyan; Jiang, Tao; Tan, Zhijun; Zhao, Chunxia; Zheng, Guanchao; Li, Zhaoxin; Zhai, Yuxiu

    2017-07-01

    In this study, we established a comprehensive method for simultaneous identification and quantification of tetrodotoxin (TTX) in fresh pufferfish tissues and pufferfish-based products using liquid chromatography/quadrupole-linear ion trap mass spectrometry (LC-QqLIT-MS). TTX was extracted by 1% acetic acid-methanol, and most of the lipids were then removed by freezing lipid precipitation, followed by purification and concentration using immunoaffinity columns (IACs). Matrix effects were substantially reduced due to the high specificity of the IACs, and thus, background interference was avoided. Quantitation analysis was therefore performed using an external calibration curve with standards prepared in mobile phase. The method was evaluated by fortifying samples at 1, 10, and 100 ng/g, respectively, and the recoveries ranged from 75.8%-107%, with a relative standard deviation of less than 15%. The TTX calibration curves were linear over the range of 1-1 000 μg/L, with a detection limit of 0.3 ng/g and a quantification limit of 1 ng/g. Using this method, samples can be further analyzed using an information-dependent acquisition (IDA) experiment, in the positive mode, from a single liquid chromatography-tandem mass spectrometry injection, which can provide an extra level of confirmation by matching the full product ion spectra acquired for a standard sample with those from an enhanced product ion (EPI) library. The scheduled multiple reaction monitoring method enabled TTX to be screened for, and TTX was positively identified using the IDA and EPI spectra. This method was successfully applied to analyze a total of 206 samples of fresh pufferfish tissues and pufferfish-based products. The results from this study show that the proposed method can be used to quantify and identify TTX in a single run with excellent sensitivity and reproducibility, and is suitable for the analysis of complex matrix pufferfish samples.

  15. Preparation of factor VII concentrate using CNBr-activated Sepharose 4B immunoaffinity chromatography

    OpenAIRE

    Mousavi Hosseini, Kamran; Nasiri, Saleh

    2015-01-01

    Background: Factor VII concentrates are used in patients with congenital or acquired factor VII deficiency or treatment of hemophilia patients with inhibitors. In this research, immunoaffinity chromatography was used to purify factor VII from prothrombin complex (Prothrombin- Proconvertin-Stuart Factor-Antihemophilic Factor B or PPSB) which contains coagulation factors II, VII, IX and X. The aim of this study was to improve purity, safety and tolerability as a highly purified factor VII conce...

  16. Purification of a polyclonal antibody against CD147 for ELISA using antigen-immunoaffinity chromatography

    Science.gov (United States)

    Liu, Shuangshuang; Li, Shasha; Zhang, Yang; Wang, Ye; Zhu, Yumeng; Wang, Bin; Chen, Zhi-Nan

    2017-01-01

    The immunoglobulin superfamily member CD147 is a widely expressed glycoprotein that occurs in both a membrane-spanning and soluble form. Sandwich ELISA is a powerful tool for analyzing soluble antigens. The aim of the present study was to obtain a highly specific polyclonal antibody against human CD147 that can be used for sandwich ELISA analysis. Expression of recombinant CD147 by a eukaryotic expression system was used to immunize rabbits to obtain antiserum. A highly specific polyclonal antibody that was able to detect soluble CD147 in sandwich ELISA was obtained by antigen-immunoaffinity chromatography purification. The purity of rabbit anti-CD147 polyclonal antibodies was ~99%, and ELISA analysis was able to determine the titer of the rabbit anti-CD147 polyclonal antibodies at 1:512,000. The lowest concentration of the standard CD147 antigen that the sandwich ELISA was able to detect was 31.25 pg/ml. The sandwich ELISA system was composed of anti-hepatoma HAb18 monoclonal antibodies and purified rabbit anti-CD147 polyclonal antibodies. The present study demonstrated that antigen-immunoaffinity chromatography may be a good technique for the purification of polyclonal antibodies, which may be used to detect antigen in sandwich ELISAs. PMID:28487989

  17. Immunoaffinity column clean-up and thin layer chromatography for determination of ochratoxin A in green coffee.

    Science.gov (United States)

    Santos, E A; Vargas, E A

    2002-05-01

    An immunoaffinity clean-up-based method for determining ochratoxin A (OTA) in green coffee aiming at one-dimensional thin layer chromatography (TLC) analysis was established. OTA was extracted with a mixture of methanol and aqueous sodium hydrogen carbonate solution, purified through an immunoaffinity column, separated on normal or reversed-phase (RP) TLC plates and detected and quantified by visual and densitometric analysis. The linear equation of the standard calibration curve by densitometric analysis gave R(2) > 0.999 (0.04-84 ng). The mean recovery (R) of OTA from spiked samples (1.8-109 microg kg(-1)) by densitometric and visual analyses were 98.4 and 103.8%, respectively. The relative standard deviations (RSD) for densitometric and visual analysis varied from 1.1 to 24.9% and from 0.0 to 18.8%, respectively. The RSD for naturally contaminated samples by densitometry (three levels of contamination, n = 3) varied from 11.1 to 18.1%. The correlation (R(2)) between high-performance liquid chromatography (HPLC) and densitometry, and between visual and densitometric analysis for spiked samples were > 0.99. The limit of detection (LOD) of the method was 0.5 microg kg(-1) for normal TLC. Toluene-ethyl acetate-88% formic acid (6:3:1 v/v/v) and acetonitrile-methanol-water-glacial acetic acid (35:35:29:10 v/v/v/v) were regarded as the suitable TLC solvents for eluting both standards and samples on normal and RP TLC plates, respectively. Toluene-acetic acid (99:1 v/v) was chosen as the spotting solvent among several others for giving the best sensitivity and resolution of OTA on TLC plates as well as the best recovery of OTA from standard and sample extract residues. Preliminary studies were carried out to investigate the reuse of the immunoaffinity column and the interference of caffeine in the OTA recovery.

  18. Advantages and drawbacks of immunoaffinity columns in analysis of mycotoxins in food.

    Science.gov (United States)

    Castegnaro, Marcel; Tozlovanu, Marianna; Wild, Christopher; Molinié, Anne; Sylla, Abdoulay; Pfohl-Leszkowicz, Annie

    2006-05-01

    A number of countries are setting legislations on mycotoxins. In order to reduce dispute between importing and exporting countries, the analytical data should be as comparable as possible, especially when levels are close to the regulatory limits. The present trend in the analysis of mycotoxins is to use immunoaffinity column (IAC) as a clean-up and enrichment technique, and Association of Official Analytical Chemists and European Union have validated methods which address a few food commodities. This study describes our experience using both conventional and IAC approaches in the analysis of three mycotoxins. Aflatoxins (AFs): Aflatoxin G1 has been detected by liquid-liquid partitioning methods with HPLC detection as false-positive in some maize. On IACs, this compound behaves as an AF, lowering the amount of the AFs trapped. The problem was solved using either TLC or HPLC with detection in the Kobra cell. Depending on the additives to food during the processing and cooking, the AFs might appear as an opened ring not recognised by the antibody. Fumonisins (FB): Compounds interfering with the FB's antibodies were also observed while analysing breakfast cereals leading to underestimation of FB. Ochratoxin A (OTA): Depending on the food composition and extraction techniques, OTA is underestimated with IAC in some breakfast cereals and coffee. These data strengthen the necessity to validate methods using IAC for each complex matrix.

  19. Immunoaffinity chromatography combined with tandem mass spectrometry: A new tool for the selective capture and analysis of brassinosteroid plant hormones

    Czech Academy of Sciences Publication Activity Database

    Oklešťková, Jana; Tarkowská, Danuše; Eyer, L.; Elbert, Tomáš; Marek, Aleš; Smržová, Z.; Novák, Ondřej; Fránek, M.; Zhabinskii, V.N.; Strnad, Miroslav

    2017-01-01

    Roč. 170, AUG 1 (2017), s. 432-440 ISSN 0039-9140 R&D Projects: GA MŠk(CZ) LO1204; GA ČR GA14-34792S; GA ČR GJ15-08202Y Institutional support: RVO:61389030 ; RVO:61388963 Keywords : Brassica napus * Brassinosteroids * Enzyme immunoassay * Immunoaffinity chromatography * Liquid chromatography-tandem mass spectrometry * Monoclonal antibodies Subject RIV: EB - Genetics ; Molecular Biology OBOR OECD: Analytical chemistry; Biochemical research methods (UOCHB-X) Impact factor: 4.162, year: 2016

  20. ELISA AND SOL-GEL BASED IMMUNOAFFINITY PURIFICATION OF THE PYRETHROID BIOALLETHRIN IN FOOD AND ENVIRONMENTAL SAMPLES

    Science.gov (United States)

    The peer-reviewed article describes the development of a new sol-gel based immunoaffinity purification procedure and an immunoassay for the pyrethroid bioallethrin. The immunoaffinity chromatography procedure was applied to food samples providing an efficient cleanup prior to im...

  1. 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.

    Science.gov (United States)

    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 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.

  2. IAC user manual

    Science.gov (United States)

    Vos, R. G.; Beste, D. L.; Gregg, J.

    1984-01-01

    The User Manual for the Integrated Analysis Capability (IAC) Level 1 system is presented. The IAC system currently supports the thermal, structures, controls and system dynamics technologies, and its development is influenced by the requirements for design/analysis of large space systems. The system has many features which make it applicable to general problems in engineering, and to management of data and software. Information includes basic IAC operation, executive commands, modules, solution paths, data organization and storage, IAC utilities, and module implementation.

  3. Development of immunoaffinity columns for pyraclostrobin extraction from fruit juices and analysis by liquid chromatography with UV detection.

    Science.gov (United States)

    Esteve-Turrillas, Francesc A; Mercader, Josep V; Agulló, Consuelo; Abad-Somovilla, Antonio; Abad-Fuentes, Antonio

    2011-07-29

    Pyraclostrobin belongs to a new generation of fungicides widely used to preserve high valuable crops. In the present study, three monoclonal antibodies with different affinities to this modern strobilurin have been evaluated for their usefulness in the production of immunoaffinity columns suitable for the solid-phase extraction, concentration, and clean-up of residues from food commodities. Different immunosorbents were produced and characterized in terms of antibody immobilization efficiency, immunosorbent binding capacity, optimum elution conditions, and reusability. Covalent coupling of the antibodies to Sepharose-CNBr gel took place with high yield (over 90%), whereas the immunosorbent efficacy to retain the analyte (from 28 to 68%) was shown to depend on the amount and type of antibody immobilized on the support. As a matter of fact, columns prepared with the monoclonal antibody PYs5#14 were able to selectively bound up to 53 μg of pyraclostrobin per gram of beads. Acetonitrile solutions were preferred over methanolic ones for analyte elution, and some immunosorbents could be reused at least 4-6 times provided that the amount of pyraclostrobin and the volume of sample did not overload the column. Effectiveness of the selected immunoaffinity column was evidenced by the development of an extraction procedure for pyraclostrobin residues from fruit juices and further determination by high-performance liquid chromatography with UV detection. A concentration factor of 50 times was achieved with the developed immunoaffinity column, which eventually resulted in a limit of quantification of 0.01 mg L(-1). Finally, quantitative recoveries were obtained on apple juice and red grape must samples spiked with pyraclostrobin from 0.01 to 1 mg L(-1). Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Isolation of cellular prion protein PRPC from brain homogenate and cerebrospinal fluid by immunoaffinity chromatography and structural analysis by 2-D map, immunoblot and by MS

    Czech Academy of Sciences Publication Activity Database

    Bílková, Z.; Castagna, A.; Zanusso, G.; Farinazzo, A.; Monaco, S.; Lenfeld, Jiří; Viovy, J.-L.; Righetti, P. G.

    2003-01-01

    Roč. 41, - (2003), s. S530 ISSN 1434-6621. [IFCC-FESCC European Congress of Clinical Chemistry and Laboratory Medicine žEuromedlabŽ /15./. 01.06.2003-05.06.2003, Barcelona] R&D Projects: GA ČR GA203/02/0023 Institutional research plan: CEZ:AV0Z4050913 Keywords : immunoaffinity chromatography * prion protein Subject RIV: CB - Analytical Chemistry, Separation

  5. IAC Jabola and IAC Esperança: common bean cultivars for market niches

    Directory of Open Access Journals (Sweden)

    Alisson Fernando Chiorato

    2009-01-01

    Full Text Available In Brazil, the trade of common beans with specialty grains such as Jalo, Bolinha, Jabola, Vermelho, Rajado,Branco, Pintado and Canário is still considered a niche market when compared to the carioca and black grain types.However, the cultivation of these beans has proved promising as an alternative income source for farmers, since it offers adifferentiated and more valuable product. IAC-Jabola and IAC-Esperança were developed by the Instituto AgronômicoCampinas (IAC in view of their excellent grain type, plant size and higher mean yield than the standard control Jalo Precoce.The IAC had these cultivars registered in MAPA/RNC based on results of 24 VCU trials in 2005/2006/2007, in the state of SãoPaulo. The yield of IAC Jabola was 2124 kg ha-1, 2336 kg ha-1, and 2558 kg ha-1, in the rainy, dry and winter seasons,respectively. The IAC- Esperança produced 1718 kg ha-1, 1545 kg ha-1, and 2263 kg ha-1 in the rainy, dry and winter seasons,respectively.

  6. Application of immunoaffinity columns for different food item samples preparation in micotoxins determination

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    Ćurčić Marijana

    2016-01-01

    Full Text Available In analytical methods used for monitoring of what special attention is paid to sample preparation. Therefore, the objective of this study was testing the efficiency of immunoaffinity columns (IAC that are based on solid phase extraction principles used for samples preparation in determining aflatoxins and ochratoxins. Aflatoxins and ochratoxins concentrations were determined in totally 56 samples of food items: wheat, corn, rice, barley and other grains (19 samples, flour and flour products from grain and additives for the bakery industry (7 samples, fruits and vegetables (3 samples, hazelnut, walnut, almond, coconut flour (4 samples, roasted cocoa beans, peanuts, tea, coffee (16 samples, spices (4 samples and meat and meat products (4 samples. Obtained results indicate advantage of IAC use for sample preparation based on enhanced specificity due to binding of extracted molecules to incorporated specific antibodies and rinsing the rest molecules from sample which could interfere with further analysis. Additional advantage is the usage of small amount of organic solvents and consequently decreased exposure of staff who conduct micotoxins determination. Of special interest is increase in method sensitivity since limit of quantification for aflatoxins and ochratoxins determination method is lower than maximal allowed concentration of these toxines prescribed by national rule book.

  7. Internal auditory canal (IAC) stenosis: imaging Findings

    International Nuclear Information System (INIS)

    Ortiz Jimenez, Johanna; Roa, Jose Luis; Figuero A, Ramon E

    2011-01-01

    Objectives: To describe the computed tomography (CT) and magnetic resonance (MR) findings in a patient with a diagnosis of internal auditory canal (IAC) stenosis. To describe the embryological development of the IAC structures and the natural history of IAC stenosis. Methods: A 4 year old girl presents with sensorineural hearing loss and bilateral recurrent otitis media. The temporal bone CT shows diminished left IAC diameter (less than 2 mm), right IAC absence and normal inner ear structures. These findings are pathognomonic for left IAC stenosis. The MR findings include left IAC stenosis and IAC neural structures absence secondary to aplasia of the vestibulocochlear nerve on each IAC . Results: Hypoplasia/aplasia of the vestibulocochlear nerve in association with IAC stenosis is an important consideration in the differential diagnosis of sensorineural hearing loss, as it is a relative contraindication for cochlear implant placement. Conclusions: IAC stenosis and vestibulocochlear nerve hypoplasia/aplasia must be excluded as an etiology of sensorineural hearing loss. The diagnosis can be made by CT and MR.

  8. Internal auditory canal (IAC) stenosis: Imaging findings

    International Nuclear Information System (INIS)

    Ortiz J, Johanna; Roa, Jose L; Figueroa Ramon E

    2011-01-01

    Objectives: To describe the computed tomography (CT) and magnetic resonance (MR) findings in a patient with a diagnosis of internal auditory canal (IAC) stenosis. To describe the embryological development of the IAC structures and the natural history of IAC stenosis. Methods: A 4 year old girl presents with sensorineural hearing loss and bilateral recurrent otitis media. The temporal bone CT shows diminished left IAC diameter (less than 2 mm), right IAC absence and normal inner ear structures. These findings are pathognomonic for left IAC stenosis. The MR findings include left IAC stenosis and IAC neural structures absence secondary to aplasia of the vestibulocochlear nerve on each IAC. Results: Hypoplasia/aplasia of the vestibulocochlear nerve in association with IAC stenosis is an important consideration in the differential diagnosis of sensorineural hearing loss, as it is a relative contraindication for cochlear implant placement. Conclusions: IAC stenosis and vestibulocochlear nerve hypoplasia/aplasia must be excluded as an etiology of sensorineural hearing loss. The diagnosis can be made by CT and MR.

  9. Preparation of factor VII concentrate using CNBr-activated Sepharose 4B immunoaffinity chromatography.

    Science.gov (United States)

    Mousavi Hosseini, Kamran; Nasiri, Saleh

    2015-01-01

    Factor VII concentrates are used in patients with congenital or acquired factor VII deficiency or treatment of hemophilia patients with inhibitors. In this research, immunoaffinity chromatography was used to purify factor VII from prothrombin complex (Prothrombin- Proconvertin-Stuart Factor-Antihemophilic Factor B or PPSB) which contains coagulation factors II, VII, IX and X. The aim of this study was to improve purity, safety and tolerability as a highly purified factor VII concentrate. PPSB was prepared using DEAE-Sephadex and was used as the starting material for purification of coagulation factor VII. Prothrombin complex was treated by solvent/detergent at 24°C for 6 h with constant stirring. The mixture of PPSB in the PBS buffer was filtered and then chromatographed using CNBr-activated Sepharose 4B coupled with specific antibody. Factors II, IX, VII, X and VIIa were assayed on the fractions. Fractions of 48-50 were pooled and lyophilized as a factor VII concentrate. Agarose gel electrophoresis was performed and Tween 80 was measured in the factor VII concentrate. Specific activity of factor VII concentrate increased from 0.16 to 55.6 with a purificationfold of 347.5 and the amount of activated factor VII (FVIIa) was found higher than PPSB (4.4-fold). RESULTS of electrophoresis on agarose gel indicated higher purity of Factor VII compared to PPSB; these finding revealed that factor VII migrated as alpha-2 proteins. In order to improve viral safety, solvent-detergent treatment was applied prior to further purification and nearly complete elimination of tween 80 (2 μg/ml). It was concluded that immuonoaffinity chromatography using CNBr-activated Sepharose 4B can be a suitable choice for large-scale production of factor VII concentrate with higher purity, safety and activated factor VII.

  10. Performance of new Hevea clones from IAC 400 series Perfomance de novos clones de Hevea da série IAC 400

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    Paulo de Souza Gonçalves

    2007-06-01

    Full Text Available The Hevea breeding program of Instituto Agronômico de Campinas (IAC has completed clonal evaluation on the following series: IAC 100, IAC 200 and IAC 300. The performance of 22 clones of Hevea brasiliensis (Willd. ex Adr. de Juss. Muell.-Arg., evolved at IAC, over a period of eleven years was evaluated in the Western Central part of the São Paulo State, Brazil. Among these 22 new clones, six were intraspecific hybrid clones (IAC 400, IAC 404, IAC 405, IAC 406, IAC 410, IAC 412 and the remaining are primary those resulted from selected ortets within half-sib progenies. An old popular clone RRIM 600, of Malaysian origin, was used as the control. The trial was laid out in a randomized block design with three replications. Yield performance over a period of four years, mean girth at the 11th year, girth increment before tapping and on tapping, thermal property of natural rubber produced, bark thickness, number of latex vessel rows in seven year virgin bark, percentage incidence of tapping panel dryness, wind damage and diseases like leaf and panel anthracnose have been observed. Sixty one percent of the clones were superior in relation to the control for yield. The clone IAC 400 recorded the highest yield (97.40 g tree-1 tap-1 over four years of tapping, followed by IAC 411 (78.87 tree-1 tap-1, whereas the control clone RRIM 600 recorded 50.86 g tree-1 tap-1. All selected clones were vigorous in growth. Girth increment of these clones was average to above average. Except for IAC 423, other clones had thick virgin bark at opening ranging from 4.84 mm for IAC 401 to 6.38 mm for IAC 416. The natural rubbers from IAC clones have shown good thermal stability up to 300ºC and no differences in the thermal behavior among rubber from clones of the IAC series and the clone RRIM 600 were found in inert atmosphere.O programa de melhoramento de Hevea do Instituto Agronômico de Campinas (IAC completou a avaliação dos clones da série IAC 100, IAC 200 e IAC

  11. PRODUTIVIDADE DE CULTIVARES DE UVAS PARA SUCO SOBRE DIFERENTES PORTA-ENXERTOS IAC EM MOCOCA-SP YIELD OF JUICE GRAPE CULTIVARS GRAFTED ON SOME IAC ROOTSTOCKS

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    MAURILO MONTEIRO TERRA

    2001-08-01

    Full Text Available Estimou-se o potencial de produção de uvas das cultivares copa Concord, Isabel e Seibel 2, recomendadas para produção de suco, enxertadas sobre os porta-enxertos IAC 313 'Tropical', 'IAC 571-6', IAC 572 'Jales', e IAC 766 'Campinas', num experimento conduzido, durante seis anos, na Estação Experimental de Mococa (21º28'S, 47º01'W do Instituto Agronômico de Campinas. Para a variedade Concord, as maiores produções médias foram obtidas quando se utilizaram os porta-enxertos 'IAC 313', 'IAC 571-6' e 'IAC 572', totalizando 3,86kg/planta, 3,81kg/planta e 3,65kg/planta, respectivamente; para 'Isabel', quando se empregaram os porta-enxertos 'IAC 572', 'IAC 571-6' e 'IAC 313', somando 3,85kg/planta, 3,63kg/planta e 3,26kg/planta; para o cv. Seibel 2, quando se fez uso dos porta-enxertos 'IAC 313', 'IAC 572' e 'IAC 571-6', auferiram-se 2,61kg/planta, 2,40kg/planta e 2,10kg/planta; por outro lado, para as três variedades, o porta-enxerto de pior performance foi o 'IAC 766'. Quanto ao vigor, representado pela massa dos ramos podados ao longo dos anos, os melhores porta-enxertos para 'Concord' foram 'IAC 572' e 'IAC 313'; para 'Isabel': 'IAC 766' e 'IAC 313'; e para 'Seibel 2': 'IAC 766' e 'IAC 572'.The yield potential of juice grape cultivars, namely Concord, Isabel and Seibel 2, grafted on 'IAC 313', 'IAC 571-6', 'IAC 572' and 'IAC 766' rootstocks was studied in an experiment conducted for six years at Mococa Experimental Station (21º28'S, 47º01'W. Regarding Concord cultivar, the greatest mean yields were achieved when grafted on 'IAC 313', 'IAC 571-6' and 'IAC 572'rootstocks, respectively 3.86kg/plant, 3.81 kg/plant and 3.65 kg/plant. 'Isabel' gave the largest grape productions when grafted on 'IAC 572' (3.85kg/plant, 'IAC 571-6' (3.63kg/plant and 'IAC 313' (3.26kg/plant. The best grape yields of 'Seibel-2' were obtained when it was grafted on 'IAC 313', 'IAC 572' and 'IAC 571-6', being respectively 2.61kg/plant, 2.40 kg/plant and 2.10 kg

  12. Industrial Assessment Center (IAC) Operations Manual

    Energy Technology Data Exchange (ETDEWEB)

    Gopalakrishnan, Bhaskaran [West Virginia Univ., Morgantown, WV (United States); Nimbalkar, Sachin U. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Wenning, Thomas J. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Thirumaran, Kiran [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    IAC Operations Manual describes organizational model and operations of the Industrial Assessment Center (IAC), Center management activities, typical process of energy assessment, and energy assessment data for specific industry sectors.

  13. Aflatoxin M1 in milk by immunoaffinity column cleanup with TLC/HPLC determination

    Directory of Open Access Journals (Sweden)

    Shundo Luzia

    2006-01-01

    Full Text Available During 2002 and 2003, a total of 107 samples of raw, pasteurized and ultrahigh treated temperature (UHT milk commercialized in the cities of São Paulo and Marília (SP were analyzed for the presence of aflatoxin M1 (AFM1. AFM1 was detected in 79 (73.8% of milk samples, ranging from <0.02 to 0.26 mug/L.The samples were analyzed using an immunoaffinity column for cleanup and a thin layer chromatography for determining AFM1. The parameters, such as recovery, repeatibility, detection and quantification limit were evaluated to optimize this method (in-house. Based on spiked samples, the recovery values ranged from 85.83 to 73.86% at levels of 0.010-0.50 mug/L, respectively, and the relative standard deviation for repeatibility ranged from 7.73 to 2.08%. The quantification limit was 0.02 mug/L. The results of some samples analyzed by this method demonstrated a satisfatory correlation when compared with High Performance Liquid Chromatography (HPLC. In conclusion, immunoaffinity column cleanup gave excellent results for recovery, sensibility and sample through put. Despite the high rate of occurrence of AFM1 in samples in both cities, the contamination level could not be considered a serious public health hazard, according to Brazilian legislation.

  14. Identification of phosphorylated butyrylcholinesterase in human plasma using immunoaffinity purification and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Aryal, Uma K.; Lin, Chiann Tso; Kim, Jong Seo; Heibeck, Tyler H.; Wang, Jun; Qian, Weijun; Lin, Yuehe

    2012-04-20

    Paraoxon (diethyl 4-nitrophenyl phosphate) is an active metabolite of the common insecticide parathion and is acutely toxic due to the inhibition of cholinesterase (ChE) activity in the nervous systems. The Inhibition of butyrylcholinesterase (BChE) activity by paraoxon is due to the formation of phosphorylated BChE adduct, and the detection of the phosphorylated BChE adduct in human plasma can serve as an exposure biomarker of organophosphate pesticides and nerve agents. In this study, we performed immunoaffinity purification and liquid chromatography tandem mass spectrometry (LC-MS/MS) analysis for identifying phosphorylated BChE in human plasma treated by paraoxon. BChE was captured by biotinylated anti-BChE polyclonal antibodies conjugated to streptavidin magnetic beads. Western blot analysis showed that the antibody was effective to recognize both native and modified BChE with high specificity. The exact phosphorylation site of BChE was confirmed on Serine 198 by MS/MS with a 108 Da modification mass and accurately measured parent ion masses. The phosphorylated BChE peptide was also successfully detected in the immunoaffinity purified sample from paraoxon treated human plasma. Thus, immunoaffinity purification combined with mass spectrometry represents a viable approach for the detection of paraoxon-modified BChE and other forms of modified BChE as exposure biomarkers of organophosphates and nerve agents.

  15. Porta-enxertos para o cultivar Máximo IAC 138-22 de uvas de vinho em Monte Alegre do Sul, SP Rootstocks for wine grape cultivar IAC 138-22

    OpenAIRE

    Maurilo Monteiro Terra; Erasmo José Paioli Pires; Sônia Maria Bonilha Marcondes Coelho; Ilene Ribeiro da Silva Passos; Rui Ribeiro dos Santos; Celso Valdevino Pommer; André Camargo Pereira da Silva; Ivan José Antunes Ribeiro

    1990-01-01

    Em Monte Alegre do Sul, SP, efetuou-se um experimento de longa duração para observar o comportamento do cultivar IAC 138-22 (Máximo) de uvas para vinho, sobre cinco porta-enxertos: RR 101-14, 'Golia', "Ripária do Traviú', IAC 572 e IAC 313. Em oito colheitas sucessivas anuais, de 1974 a 1981, analisaram-se as produções médias de uvas por planta. Os resultados indicaram que o IAC 572' foi o melhor porta-enxerto para o IAC 138-22 'Máximo'. O IAC 313 superou o IAC 572 em um dos anos estudados. T...

  16. Porta-enxertos para o cultivar Máximo IAC 138-22 de uvas de vinho em Monte Alegre do Sul, SP Rootstocks for wine grape cultivar IAC 138-22

    Directory of Open Access Journals (Sweden)

    Maurilo Monteiro Terra

    1990-01-01

    Full Text Available Em Monte Alegre do Sul, SP, efetuou-se um experimento de longa duração para observar o comportamento do cultivar IAC 138-22 (Máximo de uvas para vinho, sobre cinco porta-enxertos: RR 101-14, 'Golia', "Ripária do Traviú', IAC 572 e IAC 313. Em oito colheitas sucessivas anuais, de 1974 a 1981, analisaram-se as produções médias de uvas por planta. Os resultados indicaram que o IAC 572' foi o melhor porta-enxerto para o IAC 138-22 'Máximo'. O IAC 313 superou o IAC 572 em um dos anos estudados. Todos os outros porta-enxertos apresentaram desempenho inferior.A long term experiment was conducted at Monte Alegre do Sul, State of São Paulo, Brazil, to study the behaviour of wine grape cultivar IAC 138-22 Máximo on five rootstocks: RR 101 14, 'Golia', "Ripária do Traviú', IAC 313 and IAC 572 The yields of eight consecutive annual harvests (from 1974 to 1981 were analysed. The results indicated that IAC 572 was the best rootstock. IAC 313 can also be used but with fair results. "Ripária do Traviú', RR 101-14 and 'Golia' are not recommended as rootstocks for IAC 138-22. Considering the row spacing (2 x 1m which allows 5,000 plants/ha, the difference between average yields of the best and the worst rootstock was 8,475kg/ha of grapes, a considerable figure for the grape grower.

  17. ANÁLISE DE AGRUPAMENTO DO IMC E DO IAC E DA RELAÇÃO IAC/IMC EM INDIVÍDUOS COM IDADE ENTRE 6 A 15 ANOS

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    Julião Soares de Souza Lima Junior

    2016-11-01

    Full Text Available Conhecer as relações entre dados antropométricos e o estado nutricional das pessoas ajuda no entendimento das tendências em uma população. Este trabalho teve o objetivo de determinar em 62 jovens com idade entre 6 a 15 anos o IMC, o IAC e a relação entre IAC/IMC e utilizar método para agrupamento dos indivíduos. Os dados foram analisados por estatística descritiva e o método de agrupamento Joining. O IMC, o IAC e a Relação IAC/IMC, apresentaram os valores médios de 18,88; 27,62 e 1,51, respectivamente. Os grupos 1 e 2 apresentaram médias maiores que a média geral dos dados para o IMC. Os grupos 2, 3 e 4 apresentaram maiores valores médios que a média geral dos dados para o IAC. Os grupos 3 e 4 com média maior que a media geral para a relação IAC/IMC. Maiores relações de IAC/IMC ocorrem para indivíduos que apresentam menores valores de IMC e os maiores de IAC. O IMC aumenta com a idade e o IAC diminui à medida que a idade aumenta.

  18. Antigen-binding properties of monoclonal antibodies reactive with EBNA1 and use in immunoaffinity chromatography.

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    Sarah J Duellman

    Full Text Available Epstein-Barr virus (EBV nuclear antigen 1 (EBNA1 was overexpressed and purified from Escherichia coli. Mouse monoclonal antibodies (mAbs were prepared that react with EBNA1. Eleven high affinity mAbs were recovered. Nine mAbs are isotype IgG (all subisotype IgG(1 and two mAbs are isotype IgM. All mAbs react strongly with EBNA1 in an ELISA assay while only one mAb (designated 1EB6 fails to react in a Western blot assay. The epitopes for these mAbs were mapped to seven different regions, providing good coverage of the entire EBNA1 protein. The mAbs had differing affinity for an EBNA1/DNA complex with four mAbs able to supershift the complex completely. All mAbs can immunoprecipitate EBNA1 from E. coli overexpressing EBNA1. A modified ELISA assay, termed ELISA-elution assay, was used to screen for mAbs that release EBNA1 in the presence of a low molecular weight polyhydroxylated compound (polyol and a nonchaotropic salt. MAbs with this property, termed polyol-responsive (PR-mAbs, allow gentle elution of labile proteins and protein complexes. Four mAbs are polyol-responsive with two showing usefulness in gentle immunoaffinity chromatography. Purification with these PR-mAbs may be useful in purifying EBNA1 complexes and elucidating EBNA1-associated proteins. This panel of anti-EBNA1 mAbs will advance the study of EBV by providing new tools to detect and purify EBNA1.

  19. Resistência de soja a insetos: VIII. IAC 78-2318, linhagem com resistência múltipla Resistance of soybean to insects: VIII. IAC 78-2318 line with multiple insect resistance

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenção

    1987-01-01

    Full Text Available Estudou-se, em comparação com outros genótipos de soja, o comportamento da linhagem IAC 78-2318, em relação à oviposição e colonização da mosca-branca Bemisia tabaci (Genn. e à área foliar consumida por besouros crisomelídeos e lagartas. Em Campinas, SP, em 1981, em casa de vegetação, submeteram-se os cultivares Santa Rosa, Paraná, BR-1, Bossier, IAC 8 e IAC 12 e as linhagens IAC 73-228, IAC 78-2318, D72-9601-1, PI 171451, PI 229358 e PI 274454 à infestação artificial de adultos da mosca-branca. IAC 78-2318, embora apresentando alto número de ovos, teve colonização baixa, próxima aos materiais mais resistentes (PI 171451 e PI 229358. Em Santo Antonio de Posse, SP, em 1985, em campo, IAC 78-2318, quando comparado com IAC 80-596-2, 'Santa Rosa', 'IAC 8' e 'IAC 11', mostrou a menor perda de área foliar devida à alimentação de coleópteros crisomelídeos, principalmente Cerotoma arcuata (Oliv. e Diphaulaca viridipennis Clark, e de lagartas, com predominância de Anticarsia gemmatalis (Hubn.. Como já havia sido registrado anteriormente baixo dano de Epinotia aporema (Wals. e de percevejos pentatomideos em IAC 78-2318, com as observações presentes essa linhagem fica caracterizada como portadora de resistência múltipla a insetos.The performance of the soybean line IAC 78-2318 in relation to oviposition and colonization by the whitefly Bemisia tabaci (Genn. and to defoliation by caterpillars and chrysomelidae was studied in comparison to other varieties. At Campinas, State of São Paulo - Brazil, in greenhouse, the cultivars Santa Rosa, Paraná, BR-1, Bossier, IAC 8 and IAC 12, and the lines IAC 73-228, IAC 78-2318, D72-9601-1, PI 171451, PI 229358 e PI 274454 were submitted to artificial infestation of whitefly adults from tomato plants highly infested. Despite the high number of eggs in the IAC 78-2318 folioles, this line had a low colonization, comparable to the more resistants lines (PI 171451 and PI 229358. At Santo

  20. Evaluation of three rootstocks on the productivity of some IAC wine grape cultivars

    OpenAIRE

    Terra, Murilo Monteiro; Pires, Erasmo José Paioli; Pettinelli Jr., Armando; Pommer, Celso Valdevino; Sabino, José Carlos; Passos, Ilene Ribeiro da Silva; Coelho, Sônia Maria Bonilha Marcondes; Silva, André Camargo Pereira da; Ribeiro, Ivan José Antunes

    1990-01-01

    Em experimentos em Tietê (oito anos) e Tatuí (seis anos), compararam-se quatro cullivares IAC de uvas para vinho: IAC 133-22 Máximo e IAC 960-9 Sanches, para os tintos, e IAC 116-31 Rainha e IAC 960-12, para os brancos. Eles foram cultivados tanto como produtor direto (sem enxertia) como enxertados sobre os porta-enxertos IAC 313 'Tropical', IAC 766 e "Ripária do Traviú'. Estudou-se o potencial produtivo desses cultivares como produtores diretos, bem como sua afinidade e produtividade sobre a...

  1. Protocols for the measurement of the F2-isoprostane, 15(S)-8-iso-prostaglandin F2α, in biological samples by GC-MS or GC-MS/MS coupled with immunoaffinity column chromatography.

    Science.gov (United States)

    Tsikas, Dimitrios; Suchy, Maria-Theresia

    2016-04-15

    Arachidonic acid, the origin of the eicosanoids family, occurs in biological samples as free acid and as ester in lipids. Free arachidonic acid is oxidized to numerous metabolites by means of enzymes including cyclooxygenase (COX). Arachidonic acid esterified to lipids is attacked by reactive oxygen species (ROS) to generate numerous oxidized arachidonic acid derivatives. Generally, it is assumed that ROS-derived arachidonic acid derivatives are distinct from those generated by enzymes such as COX. Therefore, ROS-generated eicosanoids are considered specific biomarkers of oxidative stress. However, there are serious doubts concerning a strict distinction between the enzyme-derived eicosanoids and the ROS-derived iso-eicosanoids. Prominent examples are prostaglandin F2α (PGF2α) and 15(S)-8-iso-prostaglandin F2α (15(S)-8-iso-PGF2α) which have been originally considered to exclusively derive from COX and ROS, respectively. There is convincing evidence that both COX and ROS can oxidize arachidonic acid to PGF2α and 15(S)-8-iso-PGF2α. Thus, many results previously reported for 15(S)-8-iso-PGF2α as exclusive ROS-dependent reaction product, and consequently as a specific biomarker of oxidative stress, require a careful re-examination which should also consider the analytical methods used to measure 15(S)-8-iso-PGF2α. This prominent but certainly not the only example underlines more than ever the importance of the analytical chemistry in basic and clinical research areas of oxidative stress. In the present work, we report analytical protocols for the reliable quantitative determination of 15(S)-8-iso-PGF2α in human biological samples including plasma and urine by mass spectrometry coupled to gas chromatography (GC-MS, GC-MS/MS) after specific isolation of endogenous 15(S)-8-iso-PGF2α and the externally added internal standard [3,3',4,4'-(2)H4]-15(S)-8-iso-PGF2α by immunoaffinity column chromatography (IAC). 15(S)-8-iso-PGF2α esterified to plasma lipids is

  2. Iguaçu (IAC-21 e Araguaia (IAC -22: cultivares de trigo de sequeiro para o Estado de São Paulo Iguaçu (IAC 21 and Araguaia (IAC 22: wheat cultivars for upland conditions of the State of São Paulo, Brazil

    Directory of Open Access Journals (Sweden)

    João Carlos Felício

    1985-01-01

    Full Text Available Em experimentos localizados nas principais regiões tritícolas paulistas, comparou-se a produtividade e as reações aos agentes de ferrugem-do-colmo e da-folha, bem como as qualidades industriais de panificação de dois novos cultivares de trigo - Iguaçu (IAC-21 e Araguaia (IAC-22 - provenientes de cruzamentos artificiais e obtidos por seleção por método genealógico, com os cultivares BH-1146 e Maringá (IAC-5. A produção média de grãos do 'Iguaçu' foi 8% e 12% estatisticamente superior respectivamente aos cultivares testemunhas, e o 'Araguaia' superou-os em 5 e 14%. Os novos cultivares apresentaram, ao longo dos cinco anos de estudo, menores níveis de infecção de ferrugem-do-colmo (Puccinia gramínis f, sp. tritici que as testemunhas, sobressaindo-se o 'Araguaia', com baixíssimos níveis de infecção. Os novos cultivares, bem como as testemunhas, mostraram reações médias para ferrugem-da-folha. Nos ensaios de panificação a farinha do 'Araguaia', de maneira geral, exibiu melhor potencial panificável que a do Iguaçu, sendo ambas levemente superiores à farinha de trigo comercial.Two new selected germoplasms of wheat (Iguaçu and Araguaia were tested against two commercial varieties (BH-1146 and IAC-5 for yield and resistance to stem and leaf rusts in several experiments carried out in different locations of the wheat areas of the State of São Paulo, Brazil, in the period 1978-1982. Cultivar Iguaçu produced 8% and 12% more grain per hectare in comparison with respectively, cultivars BH-1146 and IAC-5; cultivar Araguaia had, respectively, 5% and 14% more grain yield than the same commercial varieties. Iguaçu and Araguaia cultivars presented less stem rust infection than BH-1146 and IAC-5 while Araguaia had a lower infection level than Iguaçu under field conditions. It was not observed differences in resistance to leaf rust among them. Araguaia exhibited better bread qualities than Iguaçu but both showed better

  3. Sensitive measurement of serum 1α,25-dihydroxyvitamin D by liquid chromatography/tandem mass spectrometry after removing interference with immunoaffinity extraction.

    Science.gov (United States)

    Yuan, Chao; Kosewick, Justin; He, Xiang; Kozak, Marta; Wang, Sihe

    2011-05-15

    Vitamin D plays important roles in bone health and a variety of other pathophysiological conditions. 1α,25-Dihydroxyvitamin D is the active form of vitamin D. Quantification of serum 1α,25-dihydroxyvitamin D is useful for evaluation of several diseases including chronic renal failure, hypoparathyroidism, sarcoidosis, and rickets. Measurement of 1α,25-dihydroxyvitamin D is very challenging due to its low circulating concentration and presence of interfering substances in serum. In this report, a liquid chromatography/tandem mass spectrometry (LC/MS/MS) method for quantifying serum 1α,25-dihydroxyvitamin D is described. Lithium adducts of 1α,25-dihydroxyvitamin D were formed prior to mass spectrometry analysis to improve ionization efficiency. We tested a number of different sample preparation procedures and found that immunoaffinity extraction was the method of choice because it completely removed isobaric interferences and matrix effects present in patient serum. Extraction efficiency, expressed as absolute recovery, was greater than 60% in both patient serum and charcoal-stripped serum. This method was linear from 3.4 to 206.2 pg/mL for 1α,25-dihydroxyvitamin D(3) and 3.9 to 212.6 pg/mL for 1α,25-dihydroxyvitamin D(2) with an accuracy of 89.8-98.4% and 97.5-115.7%, respectively. Inter-assay and intra-assay coefficients of variance (CVs) for both analytes at two different concentration levels ranged from 2.5-7.0%. Comparison with a radioimmunoassay for measuring total 1α,25-dihydroxyvitamin D concentration using 40 patient samples showed a Deming regression slope of 0.751, a y-intercept of 0.84 pg/mL, an r value of 0.7909, and a mean percentage difference of -27.1%. Comparison with a reference LC/MS/MS method (n = 20) showed a Deming regression slope of 1.020, a y-intercept of 1.32 pg/mL, an r value of 0.9797, and a mean percentage difference of -2.9%. In conclusion, usage of immunoaffinity extraction enabled a sensitive LC/MS/MS method for

  4. O pessegueiro no sistema de pomar compacto: VI. Frutificação efetiva e raleio químico em seleções IAC The peach meadow orchard system: VI. Fruit set and chemical thinning in IAC subtropical selections

    Directory of Open Access Journals (Sweden)

    Wilson Barbosa

    1992-01-01

    Full Text Available Verificou-se o potencial de frutificação e o efeito da pulverização de uréia a 12%, no raleio de frutos, em cinco pessegueiros e duas nectarineiras, cultivados em pomar compacto, na Estação Experimental de Monte Alegre do Sul (22°41'S. e 46°43'W., do Instituto Agronômico de Campinas (IAC. Dos cultivares e seleções pesquisados, 'Talismã', IAC 6782-83, IAC N 2680-91, 'Aurora-2' e IAC 282-24 apresentaram as maiores taxas de frutificação natural, a saber: 60,9; 54,2; 44,6; 41,4 e 40,0% respectivamente. A uréia a 12%, pulverizada na plena floração, mostrou-se efetiva no raleio dos frutos, reduzindo as frutificações para a faixa de 12-17%, considerada adequada para pessegueiros e nectarineiras sob altas densidades de plantio. O número médio de pêssegos e nectarinas remanescentes por ramo foi, respectivamente, de 1,1; 1,6; 1,8; 1,9; 2,0; 2,6 e 3,2 para IAC 280-28; IAC 6782-83; 'Aurora-2'; IAC 282-24; IAC N 1880-76; IAC N 2680-91 e Talismã'. A produtividade não foi prejudicada pela ação raleadora da uréia a 12%. As plantas em que permaneceram até dois frutos em média, por ramo, apresentaram produtos de melhor padrão.This paper reports the fruit set potential and effects of 12% urea on fruit drop in peach and nectarine selections in meadow orchard (5,000 plants per hectare. The experimental plot was located at the Estação Experimental of Monte Alegre do Sul (22°41'S. and 46°43'W. of the Instituto Agronômico (IAC, State of São Paulo, Brazil, which has a record of 40 hours per year with temperature bellow 7°C. The best fruit set was obtained by Talismã', IAC 6782-83, IAC N 2680-91, 'Aurora-2' and IAC 282-24, showing 60.9, 54.2, 44.6, 41.4 and 40.0% respectively. The urea 12%, sprayed at full bloom stage, significantly decreased fruit set to 12-17%. The average fruit number remaining per branch was, respectively: 1.1, 1.6, 1.8, 1.9, 2.0, 2.6 and 3.2 for IAC 280-28, IAC 6782-83, 'Aurora-2', IAC 282-24, IAC N 1880

  5. Development of a multiple immunoaffinity column for simultaneous determination of multiple mycotoxins in feeds using UPLC-MS/MS.

    Science.gov (United States)

    Hu, Xiaofeng; Hu, Rui; Zhang, Zhaowei; Li, Peiwu; Zhang, Qi; Wang, Min

    2016-09-01

    A sensitive and specific immunoaffinity column to clean up and isolate multiple mycotoxins was developed along with a rapid one-step sample preparation procedure for ultra-performance liquid chromatography-tandem mass spectrometry analysis. Monoclonal antibodies against aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, zearalenone, ochratoxin A, sterigmatocystin, and T-2 toxin were coupled to microbeads for mycotoxin purification. We optimized a homogenization and extraction procedure as well as column loading and elution conditions to maximize recoveries from complex feed matrices. This method allowed rapid, simple, and simultaneous determination of mycotoxins in feeds with a single chromatographic run. Detection limits for these toxins ranged from 0.006 to 0.12 ng mL(-1), and quantitation limits ranged from 0.06 to 0.75 ng mL(-1). Concentration curves were linear from 0.12 to 40 μg kg(-1) with correlation coefficients of R (2) > 0.99. Intra-assay and inter-assay comparisons indicated excellent repeatability and reproducibility of the multiple immunoaffinity columns. As a proof of principle, 80 feed samples were tested and several contained multiple mycotoxins. This method is sensitive, rapid, and durable enough for multiple mycotoxin determinations that fulfill European Union and Chinese testing criteria.

  6. Descrição, produtividade e estabilidade da cultivar de soja IAC-23, resistente a insetos Description, yield and stability of early soybean insect resistant cultivar IAC-23

    Directory of Open Access Journals (Sweden)

    Manoel Albino Coelho de Miranda

    2003-01-01

    Full Text Available A cultivar de soja IAC-23 foi obtida pelo método genealógico modificado, a partir do cruzamento BR-6 X IAC 83-23, tendo sido avaliada com a designação IAC 93-345, em 14 ambientes, nos Estados de São Paulo e de Minas Gerais. Os ensaios finais foram desenvolvidos em Conceição das Alagoas (MG, Mococa (SP e Campinas (SP, em 1994/95; em Conceição das Alagoas, Campinas, Morro Agudo (SP e Tarumã (SP em 1995/96; Conceição das Alagoas, Mococa, Campinas, Morro Agudo, Tarumã e Ribeirão Preto (SP, em 1996/97; e em Campinas em 1998/99. Utilizou-se o delineamento de blocos ao acaso, com quatro repetições. Em semeaduras de novembro, esse cultivar precoce, com período juvenil longo, floresceu aos 43 dias, após a semeadura, e suas plantas atingiram 67 cm de estatura. A duração entre a emergência das plântulas e o estádio de maturação (R-8 foi de 106 dias, dentro do grupo de maturação precoce. O rendimento médio de grãos foi de 3.017 kg.ha-1. As plantas na maturação apresentam pubescência marrom e sementes amarelas com hilo marrom. Essa cultivar apresenta resistência às doenças pústula-bacteriana (Xanthomonas campestris pv. glycines, fogo-selvagem (Pseudomonas syringae pv. tabaci, cancro-da-haste (Diaporthe phaseolorum f. sp. meridionalis e mancha-café ("soybean mosaic virus", SMV. Apresenta também resistência a insetos mastigadores e sugadores, semelhante à cultivar IAC-17 e superior à IAS-5. A produtividade e estabilidade apresentadas pela cultivar IAC-23 sugerem sua indicação para condições edafoclimáticas similares às dos experimentos realizados.The breeding line IAC 93-345(IAC-23 was selected from the cross BR-6 XIAC 83-23 through single seed descent method (SSD to increase insect resistance, and was evaluated at fourteen environments at São Paulo (SP and Minas Gerais (MG States: Conceição das Alagoas (MG, Mococa and Campinas (SP (1994/95; in Conceição das Alagoas, Mococa, Campinas, Morro Agudo, Tarumã and

  7. Employing immuno-affinity for the analysis of various microbial metabolites of the mycotoxin deoxynivalenol.

    Science.gov (United States)

    Zhu, Yan; Hassan, Yousef I; Shao, Suqin; Zhou, Ting

    2018-06-29

    Deoxynivalenol (DON) is a type B trichothecene mycotoxin that is commonly detected in grains infested with Fusarium species. The maximum tolerated levels of DON in the majority of world's countries are restricted to 0.75 mg kg -1 within the human food chain and to less than 1-5 mg kg -1 in animal feed depending on the feed material and/or animal species due to DON's short and long-term adverse effects on human health and animal productivity. The ability to accurately analyze DON and some of its fungal/bacterial metabolites is increasingly gaining a paramount importance in food/feed analysis and research. In this study, we used the immuno-affinity approach to enrich and detect DON and three of its bacterial metabolites, namely 3-epi-DON, 3-keto-DON, and deepoxy-DON (DOM-1). The optimized enrichment step coupled with high performance liquid chromatography can accurately and reproducibly quantify the aforementioned metabolites in feed matrixes (silage extract as an example in this case). It minimizes any background interface and provides a fast and easy-to-operate protocol for the analytical determination of such metabolites. More importantly, the presented data demonstrates the ability of the utilized monoclonal antibody, generated originally to capture DON in Enzyme-Linked Immunosorbent Assays (ELISA), to cross react with three less/non-toxic DON metabolites. This raises the concerns about the genuine need to account for such cross-reactivity when DON contamination is assessed through an immuno-affinity based analyses using the investigated antibody. Crown Copyright © 2018. Published by Elsevier B.V. All rights reserved.

  8. Porta-enxertos para o cultivar Máximo IAC 138-22 de uvas de vinho em Monte Alegre do Sul, SP

    OpenAIRE

    Terra, Maurilo Monteiro; Pires, Erasmo José Paioli; Coelho, Sônia Maria Bonilha Marcondes; Passos, Ilene Ribeiro da Silva; Santos, Rui Ribeiro dos; Pommer, Celso Valdevino; Silva, André Camargo Pereira da; Ribeiro, Ivan José Antunes

    1990-01-01

    Em Monte Alegre do Sul, SP, efetuou-se um experimento de longa duração para observar o comportamento do cultivar IAC 138-22 (Máximo) de uvas para vinho, sobre cinco porta-enxertos: RR 101-14, 'Golia', "Ripária do Traviú', IAC 572 e IAC 313. Em oito colheitas sucessivas anuais, de 1974 a 1981, analisaram-se as produções médias de uvas por planta. Os resultados indicaram que o IAC 572' foi o melhor porta-enxerto para o IAC 138-22 'Máximo'. O IAC 313 superou o IAC 572 em um dos anos estudados. T...

  9. Melhoramento do algodoeiro no Estado de São Paulo: obtenção da cultivar IAC 21

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    CIA EDIVALDO

    2001-01-01

    Full Text Available Neste trabalho é relatado o esquema utilizado para obtenção da cultivar IAC 21 realizado durante o período de 1981/82 a 1993/94. A cultivar foi originada por resseleção da IAC 19, direcionada principalmente para resistência a Colletotrichum gossypii var. cephalosporioides e nematóides, através do melhoramento genealógico. No início dos estudos as seleções e respectivas progênies foram comparadas à cultivar original IAC 19 e, posteriormente, a 'IAC 20'. Além das características econômicas de produção e qualidade da fibra, a linhagem foi avaliada para resistência múltipla às doenças: murchas de Fusarium e Verticillium, mancha-angular, ramulose e nematóides. A cultivar IAC 21 foi superior a 'IAC 19' em 6,2%, em produtividade, na média geral dos experimentos, chegando a 18,1% em solos altamente infectados por patógenos; 4,6% em produção de sementes, 2,4% em tenacidade da fibra e 6,9% em tenacidade do fio, sem perdas significativas em outras características, com exceção da porcentagem de fibra que decresceu 2,6%. Com respeito às doenças, apresentou melhores índices para murcha de Fusarium e ramulose mantendo-se, entretanto, no mesmo nível para as demais. Estudos preliminares mostraram que 'IAC 21' apresentou índices inferiores a 'CNPA ITA 90' para a anomalia "murchamento avermelhado". Devido às vantagens verificadas em relação a 'IAC 19' e 'IAC 20', 'IAC 21' foi recomendada para plantio em todas as áreas do Estado de São Paulo, excluindo-se as de ocorrência do "murchamento avermelhado".

  10. No direct effects of resistant soybean cultiva IAC-24 on Podisus nigrispinus (Heteroptera: Pentatomidae Efectos no directos de resistencia del cultivar de soya IAC-24 sobre Podisus nigrispinus (Heteroptera: Pentatomidae

    Directory of Open Access Journals (Sweden)

    José Cola Zanuncio

    2012-12-01

    Full Text Available The parameters of survival, development and reproduction of Podisus nigrispinus Dallas, 1851 (Heteroptera: Pentatomidae may be affected by feeding on soybean (Glycine max L. Merr.; Fabaceae cultivars. The direct effect was evaluated of the insect-resistant soybean 'IAC-24' (insect-susceptible soybean 'UFVS-2006' + pupae of Tenebrio molitor L., 1758 Coleoptera: Tenebrionidae versus 'IAC-24' plants + pupae of T. molitor in the nymph and adult stages of the predator P. nigrispinus. The duration of the nymph stage was similar between treatments, but 'IAC-24' reduced the duration of the IV instar of this predator. The survival of P. nigrispinus was similar between treatments in the instars I, II, IV and V and in the nymph stage, but the survival of the III instar was longer with 'IAC-24' plants. The body mass of nymphs in the first day of the III, IV, and V instars after ecdysis and newly emerged adults; reproductive characteristics (periods of pre-oviposition, oviposition, post-oviposition and egg incubation; egg laying interval, number of egg masses per female, nymphs per female, nymphs per egg mass and percentage of nymphs hatching and life span of males and females of P. nigrispinus were similar between treatments. The resistant soybean 'IAC-24' showed no direct deleterious effects on P. nigrispinus, which implies its innocuity and compatibility with this predator.Los par ámetros de supervivencia, desarrollo y reproducción de Podìsus nìgrìspìnus Dallas, 1851 (Heteroptera: Pentatomidae pueden verse afectados por la alimentación en cultivos de soya (Glycìne max L. Merr.; Fabaceae. Se evaluó el efecto directo de la soya 'IAC-24' resistente a insectos (soya 'UFVS-2006' susceptible a insectos + pupas de Tenebrìo molìtor L., 1758 Coleoptera: Tenebrionidae vs. plantas 'IAC-24' + pupas de T. molìtor sobre los estados de ninfa y adulto del depredador P. nìgrìspìnus. La duración del estado ninfal fue similar entre tratamientos, no obstante

  11. Simultaneous detection of airborne aflatoxin, ochratoxin and zearalenone in a poultry house by immunoaffinity clean-up and high-performance liquid chromatography.

    Science.gov (United States)

    Wang, Yaling; Chai, Tongjie; Lu, Guozhong; Quan, Chunsan; Duan, Huiyong; Yao, Meiling; Zucker, Bert-Andree; Schlenker, Gerd

    2008-06-01

    An AOZ method, based on high-performance liquid chromatography (HPLC), was optimized on HPLC condition such as mobile phase and wavelength to simultaneously quantify six kinds of mycotoxins [four aflatoxins (AFs), ochratoxin A (OTA) and zearalenone (ZEA)]. Conditions for immunoaffinity clean-up, HPLC and photo-derivatization were optimized in this study and successfully applied in assessment of airborne mycotoxins from a poultry house in Dalian, China. Fifty-two air samples were collected with AGI-30 air samplers using pure water as collection media. Twenty air samples (20/52, 38.46%) were positive for four toxins. Among the positive samples, airborne mycotoxin concentrations (mean+/-S.D.) for AFG(2), AFB(1), and ZEA were 0.189+/-0.024 (n=9), 0.080+/-0.003 (n=11) and 2.363+/-0.030 (n=5)ng/m(3) air, while the concentration for OTA was 8.530 (n=1)ng/m(3). No positive sample was found for either AFG(1) or AFB(2). A chicken may inhale 0.019-0.057 ng AFG(2), 0.013-0.019 ng AFB(1), 0.436-0.513 ng ZEA, and 1.706 ng OTA, respectively, in a day. A poultry worker may inhale 0.504-1.512 ng AFB(1), 0.752-2.28 ng AFG(2), 68.240 ng OTA, and 17.432-20.512 ng ZEA in a working day. This is the first report on airborne mycotoxins in poultry house. These data may have importance in animal and public health implications.

  12. Natural occurrence of ochratoxin A in wolfberry fruit wine marketed in China.

    Science.gov (United States)

    Kuang, Ying; Qiu, Feng; Kong, Weijun; Yang, Meihua

    2012-01-01

    Wolfberry fruit wine (WFW) is widely used as a global functional food to improve the immune system and prevent human disease. A total of 36 bottled WFWs were randomly collected in China between 2005 and 2010. Samples were analysed for the presence of ochratoxin A (OTA) using immunoaffinity column (IAC) clean-up and high-performance liquid chromatography with fluorescence detection (HPLC-FLD). Positive results were confirmed by liquid chromatography-electrospray ionisation-tandem mass spectrometry (LC-ESI-MS/MS). The limit of detection (LOD), based on a signal-to-noise ratio of 3, was 0.05 ng mL⁻¹. Recoveries ranged from 78.3% to 94.7% and relative standard deviations from 1.1% to 4.3% within the spiking range of 0.2-20 ng mL⁻¹. OTA was detected in one sample, below the maximum allowable limit as established by the European community.

  13. Plantio direto de mamona 'IAC 80' com culturas alimentares No tillage of castor bean 'IAC 80' with food crops

    Directory of Open Access Journals (Sweden)

    Antonio Carlos Pries Devide

    2010-06-01

    Full Text Available Avaliou-se o desempenho da mamona 'IAC 80' cultivada em fileiras duplas, no espaçamento 4,0 x (1,0 x 1,0 m em plantio direto na palha da aveia branca; consorciada com culturas alimentares. O cereal foi utilizado para a produção de grãos (1.375 kg ha-1 e cobertura do solo (1.593 kg ha-1 MS; ciclagem de 35 kg K ha-1. Os consortes foram semeados nas entrelinhas duplas de mamona (Ma: Ma + milho; Ma + feijão; Ma + milho + feijão e Ma + milho + abóbora. Apesar de suscetível ao mofo cinzento, a IAC 80 produziu 1.060 kg ha-1 de grãos; do milho foram colhidas 22.542 espigas verdes ha-1 (5.333 kg ha-1 significando um aporte de 3,15 t ha-1 MS (39 kg N ha-1; 58 kg K ha-1. A abóbora e o feijão não produziram colheitas comerciais. O sistema contendo aveia, mamona e milho, apresentou produtividade satisfatória, contribuindo para a produção de bioenergia com segurança alimentar e conservação ambiental.The objective of this study was to evaluate the performance of castor bean 'IAC 80' grown in double rows spaced at 4.0 x (1.0 x 1.0 m in no-tillage in the white oat straw, intercropped with food crops. The cereal was used for grain production (1375 kg ha-1 and soil coverage (1593 kg ha-1 MS; cycling of 35 kg K ha-1. The associated cultivation was double seeded between the lines of castor beans (Ma: Ma + corn, beans + Ma, Ma + beans and maize corn Ma + pumpkin. The cv. IAC 80, though susceptible to gray mold, produced 1060 kg ha-1 grain; corn ears were harvested with 22.542 ha-1 (5.333 kg ha-1, meaning an input of 3.15 t ha-1 MS (39 kg N ha-1, 58 kg K ha-1. Pumpkin and bean crops did not yield commercial crops. The system containing oats, castor beans, and corn yielded satisfactory and contributed to the production of bioenergy with food security and environmental conservation.

  14. Desempenho de clones de seringueira da série IAC 300 selecionados para a região noroeste do Estado de São Paulo Performance of Hevea clones from IAC 300 series selected in the northwestern region of São Paulo State, Brazil

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    Paulo de Souza Gonçalves

    2001-04-01

    Full Text Available É apresentado o desempenho de 19 novos clones de seringueira [Hevea brasiliensis (Willd. exAdr. de Juss. Muell. Arg.], resultantes de hibridações conduzidas no Instituto Agronômico e avaliados em experimento de pequena escala, tendo o clone RRIM 600 como testemunha. O experimento em campo obedeceu ao delineamento em blocos ao acaso, com três repetições. Com relação à produção de borracha seca, o clone IAC 40 apresentou a maior média (62,22 g/árvore/sangria nos três anos de avaliação, seguido pelo IAC 301 (57,67 g/árvore/sangria e pelo IAC 300 (50,61 g/árvore/sangria, com produções 154%, 138% e 123% superiores em relação ao RRIM 600 (41,04 g/árvore/sangria. Todos os clones selecionados foram vigorosos, com perímetro do caule na abertura do painel variando de 37,81 cm (IAC 317 a 50,90 cm (IAC 315. A porcentagem de plantas aptas a sangria variou de 20,0% (IAC 317 a 100% (IAC 315. Todos os clones apresentaram baixas incidências de quebra pelo vento e de secamento do painel. Não foi detectada nenhuma doença foliar em caráter epidêmico. Dos clones estudados, 15 apresentaram alta resistência à antracnose do painel, e foram superiores ao RRIM 600; os outros cinco apresentaram resistência moderada semelhante ao RRIM 600.The present paper shows the performance of 19 rubber tree [Hevea brasiliensis (Willd. ex Adr. de Juss. Muell. Arg.] originated from Hevea breeding programme conducted at the Instituto Agronômico de Campinas (IAC and evaluated in a small scale trial in the northwestern of São Paulo State, Brazil. The old popular clone RRIM 600 of Malaysian origin was used as control. The trial was laid out in a randomized block design with three replications. Concerned to yielding the clone IAC 40 recorded highest yield (62.22 g/tree/tap over three years of tapping which was followed by IAC 301 (57.67 g/tree/tap and IAC 300 (50.61 g/tree/tap yielding 154%, 138% and 123% superior to the control clone and RRIM 600 whereas

  15. pre-germination treatments in castor seeds, cultivar IAC 226

    International Nuclear Information System (INIS)

    Costa Nobre, Danubia Aparecida; Gomes Damascena, Joyce; Marcia, Andreia; Santos de Souza, David; Pereira dos Santos, Marlucia; Rodrigues Pereira, Adriana; Goncalves Pereira, Cassio

    2013-01-01

    The present study aimed to evaluate the efficiency of different pre-germination treatments in castor beans, IAC 226. The experimental design was completely randomized in a factorial 4 x 4 (four temperatures and four immersion times), with four replications. Pre-germination treatments were: immersion in water at room temperature (25 Celsius degrade) and immersion in hot water at temperatures of 60, 70 and 80 Celsius degrade for 2, 4, 6 and 8 minutes. Water content of the seeds was determined before treatments. Before and after each treatment, seeds were subjected to germination test; 20-30 Celsius degrade alternating temperature, determining the percentages of normal and abnormal seedlings, dormant and dead seeds. Independent of time, immersion in 70 Celsius degrade, water was the most efficient treatment for accelerating germination of castor bean cultivar IAC 226.

  16. Chromatographic Monoliths for High-Throughput Immunoaffinity Isolation of Transferrin from Human Plasma

    Directory of Open Access Journals (Sweden)

    Irena Trbojević-Akmačić

    2016-06-01

    Full Text Available Changes in protein glycosylation are related to different diseases and have a potential as diagnostic and prognostic disease biomarkers. Transferrin (Tf glycosylation changes are common marker for congenital disorders of glycosylation. However, biological interindividual variability of Tf N-glycosylation and genes involved in glycosylation regulation are not known. Therefore, high-throughput Tf isolation method and large scale glycosylation studies are needed in order to address these questions. Due to their unique chromatographic properties, the use of chromatographic monoliths enables very fast analysis cycle, thus significantly increasing sample preparation throughput. Here, we are describing characterization of novel immunoaffinity-based monolithic columns in a 96-well plate format for specific high-throughput purification of human Tf from blood plasma. We optimized the isolation and glycan preparation procedure for subsequent ultra performance liquid chromatography (UPLC analysis of Tf N-glycosylation and managed to increase the sensitivity for approximately three times compared to initial experimental conditions, with very good reproducibility. This work is licensed under a Creative Commons Attribution 4.0 International License.

  17. Affinity monolith chromatography: A review of general principles and applications.

    Science.gov (United States)

    Li, Zhao; Rodriguez, Elliott; Azaria, Shiden; Pekarek, Allegra; Hage, David S

    2017-11-01

    Affinity monolith chromatography, or AMC, is a liquid chromatographic method in which the support is a monolith and the stationary phase is a biological-binding agent or related mimic. AMC has become popular for the isolation of biochemicals, for the measurement of various analytes, and for studying biological interactions. This review will examine the principles and applications of AMC. The materials that have been used to prepare AMC columns will be discussed, which have included various organic polymers, silica, agarose, and cryogels. Immobilization schemes that have been used in AMC will also be considered. Various binding agents and applications that have been reported for AMC will then be described. These applications will include the use of AMC for bioaffinity chromatography, immunoaffinity chromatography, dye-ligand affinity chromatography, and immobilized metal-ion affinity chromatography. The use of AMC with chiral stationary phases and as a tool to characterize biological interactions will also be examined. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Occurrence of ochratoxin A in wine and beer samples from China.

    Science.gov (United States)

    Wu, Jianwei; Tan, Yinfeng; Wang, Yuqi; Xu, Rong

    2011-01-01

    A total of 125 wine and beer samples, including 42 white, 63 red wine and 20 beer samples, originating from several areas of China were analyzed for ochratoxin A (OTA). An analytical method based on immunoaffinity column (IAC) for clean-up and high performance liquid chromatography with fluorescence detection (HPLC-FD) was used to determine OTA. Positive results were further confirmed by LC-MS-MS. OTA was detected in 22 (17.6%) samples at levels of 0.02-1.18 ng/ml, which were below the EU maximum limit. The mean OTA concentration in red wine was slightly higher than in white wine. This study showed that OTA occurs in wine and beer in China but at levels that pose no danger of significant human exposure to OTA from this source.

  19. Evaluation of natural rubber from IAC series clones by solid state {sup 13}C NMR; Avaliacao da borracha natural de clones da serie IAC por {sup 13}C RMN no estado solido

    Energy Technology Data Exchange (ETDEWEB)

    Martins, Maria A.; Moreno, Rogerio M.B.; Goncalves, Paulo S. [Instituto Agronomico de Campinas, SP (Brazil). Centro de Cafe e Plantas Tropicais. Programa Seringueira]. E-mails: paulog@iac.sp.gov.br; mariaalice@cnpdia.embrapa.br; Forato, Lucimara A.; Colnago, Luiz A.; Mattoso, Luiz H.C. [EMBRAPA Instrumentacao Agropecuaria, Sao Carlos, SP (Brazil)]. E-mail: colnago@cnpdia.embrapa.br; forato@cnpdia.embrapa.br; rogerio@cnpdia.embrapa.br; mattoso@cnpdia.embrapa.br; Job, Aldo E. [Universidade Estadual Paulista (UNESP), Presidente Prudente, SP (Brazil). Departamento de Fisica, Quimica e Biologia

    2005-07-01

    Agronomic Institute (IAC) and EMBRAPA Agricultural Instrumentation (EMBRAPA/CNPDIA) have been studied Hevea species in order to increase the production of the natural rubber and to develop new clones more appropriated to Brazil's soil and climate. Structural characterization of natural rubber [Hevea brasiliensis (Willd. ex Adr. de Juss.) Muell. - Arg.] from new clones of the IAC series (IAC 300, 301, 302, 303, 35, 40, and 56) and from RRIM 600 clone has been studied by high-resolution solid-state {sup 13}C NMR and by single pulse technique. The results have shown that the application of solid-state {sup 13}C NMR using the single pulse technique is a powerful tool to study natural rubber. The spectra obtained through this technique confirmed that natural rubber from all clones studied are cis-1,4-polyisoprene (author) form.(author)

  20. Quantitative analysis of N-glycans from human alfa-acid-glycoprotein using stable isotope labeling and zwitterionic hydrophilic interaction capillary liquid chromatography electrospray mass spectrometry as tool for pancreatic disease diagnosis

    International Nuclear Information System (INIS)

    Giménez, Estela; Balmaña, Meritxell; Figueras, Joan; Fort, Esther; Bolós, Carme de; Sanz-Nebot, Victòria; Peracaula, Rosa; Rizzi, Andreas

    2015-01-01

    Highlights: • The method enables relative quantitation of hAGP glycans from pathological samples • Pancreatic cancer samples clearly showed an increase of hAGP fucosylated glycans. • Fucosylated glycans could be potential biomarkers for diagnosing pancreatic cancer. • The established method could be extremely useful to find novel glycoprotein biomarkers - Abstract: In this work we demonstrate the potential of glycan reductive isotope labeling (GRIL) using [ 12 C]- and [ 13 C]-coded aniline and zwitterionic hydrophilic interaction capillary liquid chromatography electrospray mass spectrometry (μZIC-HILIC-ESI-MS) for relative quantitation of glycosylation variants in selected glycoproteins present in samples from cancer patients. Human α 1 -acid-glycoprotein (hAGP) is an acute phase serum glycoprotein whose glycosylation has been described to be altered in cancer and chronic inflammation. However, it is not clear yet whether some particular glycans in hAGP can be used as biomarker for differentiating between these two pathologies. In this work, hAGP was isolated by immunoaffinity chromatography (IAC) from serum samples of healthy individuals and from those suffering chronic pancreatitis and different stages of pancreatic cancer, respectively. After de-N-glycosylation, relative quantitation of the hAGP glycans was carried out using stable isotope labeling and μZIC-HILIC-ESI-MS analysis. First, protein denaturing conditions prior to PNGase F digestion were optimized to achieve quantitative digestion yields, and the reproducibility of the established methodology was evaluated with standard hAGP. Then, the proposed method was applied to the analysis of the clinical samples (control vs. pathological). Pancreatic cancer samples clearly showed an increase in the abundance of fucosylated glycans as the stage of the disease increases and this was unlike to samples from chronic pancreatitis. The results gained here indicate the mentioned glycan in hAGP as a

  1. Site-directed immobilization of a genetically engineered anti-methotrexate antibody via an enzymatically introduced biotin label significantly increases the binding capacity of immunoaffinity columns.

    Science.gov (United States)

    Davenport, Kaitlynn R; Smith, Christopher A; Hofstetter, Heike; Horn, James R; Hofstetter, Oliver

    2016-05-15

    In this study, the effect of random vs. site-directed immobilization techniques on the performance of antibody-based HPLC columns was investigated using a single-domain camelid antibody (VHH) directed against methotrexate (MTX) as a model system. First, the high flow-through support material POROS-OH was activated with disuccinimidyl carbonate (DSC), and the VHH was bound in a random manner via amines located on the protein's surface. The resulting column was characterized by Frontal Affinity Chromatography (FAC). Then, two site-directed techniques were explored to increase column efficiency by immobilizing the antibody via its C-terminus, i.e., away from the antigen-binding site. In one approach, a tetra-lysine tail was added, and the antibody was immobilized onto DSC-activated POROS. In the second site-directed approach, the VHH was modified with the AviTag peptide, and a biotin-residue was enzymatically incorporated at the C-terminus using the biotin ligase BirA. The biotinylated antibody was subsequently immobilized onto NeutrAvidin-derivatized POROS. A comparison of the FAC analyses, which for all three columns showed excellent linearity (R(2)>0.999), revealed that both site-directed approaches yield better results than the random immobilization; the by far highest efficiency, however, was determined for the immunoaffinity column based on AviTag-biotinylated antibody. As proof of concept, all three columns were evaluated for quantification of MTX dissolved in phosphate buffered saline (PBS). Validation using UV-detection showed excellent linearity in the range of 0.04-12μM (R(2)>0.993). The lower limit of detection (LOD) and lower limit of quantification (LLOQ) were found to be independent of the immobilization strategy and were 40nM and 132nM, respectively. The intra- and inter-day precision was below 11.6%, and accuracy was between 90.7% and 112%. To the best of our knowledge, this is the first report of the AviTag-system in chromatography, and the first

  2. PHARMACEUTICAL AND BIOMEDICAL APPLICATIONS OF AFFINITY CHROMATOGRAPHY: RECENT TRENDS AND DEVELOPMENTS

    Science.gov (United States)

    Hage, David S.; Anguizola, Jeanethe A.; Bi, Cong; Li, Rong; Matsuda, Ryan; Papastavros, Efthimia; Pfaunmiller, Erika; Vargas, John; Zheng, Xiwei

    2012-01-01

    Affinity chromatography is a separation technique that has become increasingly important in work with biological samples and pharmaceutical agents. This method is based on the use of a biologically-related agent as a stationary phase to selectively retain analytes or to study biological interactions. This review discusses the basic principles behind affinity chromatography and examines recent developments that have occurred in the use of this method for biomedical and pharmaceutical analysis. Techniques based on traditional affinity supports are discussed, but an emphasis is placed on methods in which affinity columns are used as part of HPLC systems or in combination with other analytical methods. General formats for affinity chromatography that are considered include step elution schemes, weak affinity chromatography, affinity extraction and affinity depletion. Specific separation techniques that are examined include lectin affinity chromatography, boronate affinity chromatography, immunoaffinity chromatography, and immobilized metal ion affinity chromatography. Approaches for the study of biological interactions by affinity chromatography are also presented, such as the measurement of equilibrium constants, rate constants, or competition and displacement effects. In addition, related developments in the use of immobilized enzyme reactors, molecularly imprinted polymers, dye ligands and aptamers are briefly considered. PMID:22305083

  3. Immunoaffinity purification and reconstitution of the human bilirubin/phenol UDP-glucuronosyltransferase family

    NARCIS (Netherlands)

    Seppen, J.; Jansen, P. L.; Oude Elferink, R. P.

    1995-01-01

    When membrane proteins are solubilized and subjected to purification procedures, the loss of lipids surrounding the protein often results in irreversible inactivation. We describe a procedure for the immunoaffinity purification of the membrane protein UDP-glucuronosyltransferase from human liver.

  4. IMMUNOAFFINITY PURIFICATION AND RECONSTITUTION OF THE HUMAN BILIRUBIN PHENOL UDP-GLUCURONOSYLTRANSFERASE FAMILY

    NARCIS (Netherlands)

    SEPPEN, J; JANSEN, PLM; ELFERINK, RPJO

    When membrane proteins are solubilized and subjected to purification procedures, the loss of lipids surrounding the protein often results in irreversible inactivation. We describe a procedure for the immunoaffinity purification of the membrane protein UDP-glucuronosyltransferase from human liver.

  5. Optimal selection of epitopes for TXP-immunoaffinity mass spectrometry.

    Science.gov (United States)

    Planatscher, Hannes; Supper, Jochen; Poetz, Oliver; Stoll, Dieter; Joos, Thomas; Templin, Markus F; Zell, Andreas

    2010-06-25

    Mass spectrometry (MS) based protein profiling has become one of the key technologies in biomedical research and biomarker discovery. One bottleneck in MS-based protein analysis is sample preparation and an efficient fractionation step to reduce the complexity of the biological samples, which are too complex to be analyzed directly with MS. Sample preparation strategies that reduce the complexity of tryptic digests by using immunoaffinity based methods have shown to lead to a substantial increase in throughput and sensitivity in the proteomic mass spectrometry approach. The limitation of using such immunoaffinity-based approaches is the availability of the appropriate peptide specific capture antibodies. Recent developments in these approaches, where subsets of peptides with short identical terminal sequences can be enriched using antibodies directed against short terminal epitopes, promise a significant gain in efficiency. We show that the minimal set of terminal epitopes for the coverage of a target protein list can be found by the formulation as a set cover problem, preceded by a filtering pipeline for the exclusion of peptides and target epitopes with undesirable properties. For small datasets (a few hundred proteins) it is possible to solve the problem to optimality with moderate computational effort using commercial or free solvers. Larger datasets, like full proteomes require the use of heuristics.

  6. Blood coagulation factor VIII: An overview

    Indian Academy of Sciences (India)

    Unknown

    Solvent, detergent and heat treatment. Hemofil-M. Baxter. Pooled human venous plasma. Immunoaffinity chromatography using murine monoclonal anti- body. Solvent and detergent. Monarc-M. American. Red Cross. Pooled human venous plasma. Immunoaffinity chromatography using murine monoclonal antibody.

  7. Rapid Isolation of a Single-Chain Antibody against the Cyanobacterial Toxin Microcystin-LR by Phage Display and Its Use in the Immunoaffinity Concentration of Microcystins from Water

    Science.gov (United States)

    McElhiney, Jacqui; Drever, Mathew; Lawton, Linda A.; Porter, Andy J.

    2002-01-01

    A naïve (unimmunized) human semisynthetic phage display library was employed to isolate recombinant antibody fragments against the cyanobacterial hepatotoxin microcystin-LR. Selected antibody scFv genes were cloned into a soluble expression vector and expressed in Escherichia coli for characterization against purified microcystin-LR by competition enzyme-linked immunosorbent assay (ELISA). The most sensitive single-chain antibody (scAb) isolated was capable of detecting microcystin-LR at levels below the World Health Organization limit in drinking water (1 μg liter−1) and cross-reacted with three other purified microcystin variants (microcystin-RR, -LW, and -LF) and the related cyanotoxin nodularin. Extracts of the cyanobacterium Microcystis aeruginosa were assayed by ELISA, and quantifications of microcystins in toxic samples showed good correlation with analysis by high-performance liquid chromatography. Immobilized scAb was also used to prepare immunoaffinity columns, which were assessed for the ability to concentrate microcystin-LR from water for subsequent analysis by high-performance liquid chromatography. Anti-microcystin-LR scAb was immobilized on columns via a hexahistidine tag, ensuring maximum exposure of antigen binding sites, and the performance of the columns was evaluated by directly applying 150 ml of distilled water spiked with 4 μg of purified microcystin-LR. The procedure was simple, and a recovery rate of 94% was achieved following elution in 1 ml of 100% methanol. Large-scale, low-cost production of anti-microcystin-LR scAb in E. coli is an exciting prospect for the development of biosensors and on-line monitoring systems for microcystins and will also facilitate a range of immunoaffinity applications for the cleanup and concentration of these toxins from environmental samples. PMID:12406716

  8. Affinity monolith chromatography: A review of principles and recent analytical applications

    Science.gov (United States)

    Pfaunmiller, Erika L.; Paulemond, Marie Laura; Dupper, Courtney M.; Hage, David S.

    2012-01-01

    Affinity monolith chromatography (AMC) is a type of liquid chromatography that uses a monolithic support and a biologically-related binding agent as a stationary phase. AMC is a powerful method for the selective separation, analysis or studies of specific target compounds in a sample. This review discusses the basic principles of AMC and recent developments or applications of this method, with particular emphasis being given to work that has appeared in the last five years. Various materials that have been used to prepare columns for AMC are examined, including organic monoliths, silica monoliths, agarose monoliths and cryogels. These supports have been used in AMC for formats that have ranged from traditional columns to disks, microcolumns and capillaries. Many binding agents have also been employed in AMC, such as antibodies, enzymes, proteins, lectins, immobilized metal-ions and dyes. Some applications that have been reported with these binding agents in AMC are bioaffinity chromatography, immunoaffinity chromatography or immunoextraction, immobilized metal-ion affinity chromatography, dye-ligand affinity chromatography, chiral separations and biointeraction studies. Examples are presented from fields that include analytical chemistry, pharmaceutical analysis, clinical testing and biotechnology. Current trends and possible future directions in AMC are also discussed. PMID:23187827

  9. Agricultural registers for the assessment of landscape changes: Options and challenges for the application of IACS and LPIS data

    DEFF Research Database (Denmark)

    Levin, Gregor

    In the early 1990ies the Integrated Administration and Control System (IACS) was launched with the aim to support administration and payments of agricultural subsidies (EEC, 1992). IACS is based on farmers’ individual registrations and contains farm level (e.g. animal husbandry and manure...

  10. Protein Turnover Measurements in Human Serum by Serial Immunoaffinity LC-MS/MS.

    Science.gov (United States)

    Farrokhi, Vahid; Chen, Xiaoying; Neubert, Hendrik

    2018-02-01

    The half-life of target proteins is frequently an important parameter in mechanistic pharmacokinetic and pharmacodynamic (PK/PD) modeling of biotherapeutics. Clinical studies for accurate measurement of physiologically relevant protein turnover can reduce the uncertainty in PK/PD model-based predictions, for example, of the therapeutic dose and dosing regimen in first-in-human clinical trials. We used a targeted mass spectrometry work flow based on serial immunoaffinity enrichment ofmultiple human serum proteins from a [5,5,5- 2 H 3 ]-L-leucine tracer pulse-chase study in healthy volunteers. To confirm the reproducibility of turnover measurements from serial immunoaffinity enrichment, multiple aliquots from the same sample set were subjected to protein turnover analysis in varying order. Tracer incorporation was measured by multiple-reaction-monitoring mass spectrometry and target turnover was calculated using a four-compartment pharmacokinetic model. Five proteins of clinical or therapeutic relevance including soluble tumor necrosis factor receptor superfamily member 12A, tissue factor pathway inhibitor, soluble interleukin 1 receptor like 1, soluble mucosal addressin cell adhesion molecule 1, and muscle-specific creatine kinase were sequentially subjected to turnover analysis from the same human serum sample. Calculated half-lives ranged from 5-15 h; however, no tracer incorporation was observed for mucosal addressin cell adhesion molecule 1. The utility of clinical pulse-chase studies to investigate protein turnover can be extended by serial immunoaffinity enrichment of target proteins. Turnover analysis from serum and subsequently from remaining supernatants provided analytical sensitivity and reproducibility for multiple human target proteins in the same sample set, irrespective of the order of analysis. © 2017 American Association for Clinical Chemistry.

  11. Optimal selection of epitopes for TXP-immunoaffinity mass spectrometry

    Directory of Open Access Journals (Sweden)

    Joos Thomas

    2010-06-01

    Full Text Available Abstract Background Mass spectrometry (MS based protein profiling has become one of the key technologies in biomedical research and biomarker discovery. One bottleneck in MS-based protein analysis is sample preparation and an efficient fractionation step to reduce the complexity of the biological samples, which are too complex to be analyzed directly with MS. Sample preparation strategies that reduce the complexity of tryptic digests by using immunoaffinity based methods have shown to lead to a substantial increase in throughput and sensitivity in the proteomic mass spectrometry approach. The limitation of using such immunoaffinity-based approaches is the availability of the appropriate peptide specific capture antibodies. Recent developments in these approaches, where subsets of peptides with short identical terminal sequences can be enriched using antibodies directed against short terminal epitopes, promise a significant gain in efficiency. Results We show that the minimal set of terminal epitopes for the coverage of a target protein list can be found by the formulation as a set cover problem, preceded by a filtering pipeline for the exclusion of peptides and target epitopes with undesirable properties. Conclusions For small datasets (a few hundred proteins it is possible to solve the problem to optimality with moderate computational effort using commercial or free solvers. Larger datasets, like full proteomes require the use of heuristics.

  12. Quantitative analysis of N-glycans from human alfa-acid-glycoprotein using stable isotope labeling and zwitterionic hydrophilic interaction capillary liquid chromatography electrospray mass spectrometry as tool for pancreatic disease diagnosis

    Energy Technology Data Exchange (ETDEWEB)

    Giménez, Estela, E-mail: estelagimenez@ub.edu [Department of Analytical Chemistry, University of Barcelona, Diagonal 647, E-08028 Barcelona (Spain); Balmaña, Meritxell [Biochemistry and Molecular Biology Unit, Department of Biology, University of Girona, Campus Montilivi s/n, 17071 Girona (Spain); Figueras, Joan [Department of Surgery, Dr. Josep Trueta University Hospital, IdlBGi, 17007 Girona (Spain); Fort, Esther [Digestive Unit, Dr. Josep Trueta University Hospital, 17007 Girona (Spain); Bolós, Carme de [Gastroesophagic Cancer Research Group, Research Programme in Cancer, Hospital del Mar Medical Research Institute (IMIM), Dr. Aiguader, 88, 08003 Barcelona (Spain); Sanz-Nebot, Victòria [Department of Analytical Chemistry, University of Barcelona, Diagonal 647, E-08028 Barcelona (Spain); Peracaula, Rosa [Biochemistry and Molecular Biology Unit, Department of Biology, University of Girona, Campus Montilivi s/n, 17071 Girona (Spain); Rizzi, Andreas [Institute of Analytical Chemistry, University of Vienna, Währinger Straße 38, A-1090 Vienna (Austria)

    2015-03-25

    Highlights: • The method enables relative quantitation of hAGP glycans from pathological samples • Pancreatic cancer samples clearly showed an increase of hAGP fucosylated glycans. • Fucosylated glycans could be potential biomarkers for diagnosing pancreatic cancer. • The established method could be extremely useful to find novel glycoprotein biomarkers - Abstract: In this work we demonstrate the potential of glycan reductive isotope labeling (GRIL) using [{sup 12}C]- and [{sup 13}C]-coded aniline and zwitterionic hydrophilic interaction capillary liquid chromatography electrospray mass spectrometry (μZIC-HILIC-ESI-MS) for relative quantitation of glycosylation variants in selected glycoproteins present in samples from cancer patients. Human α{sub 1}-acid-glycoprotein (hAGP) is an acute phase serum glycoprotein whose glycosylation has been described to be altered in cancer and chronic inflammation. However, it is not clear yet whether some particular glycans in hAGP can be used as biomarker for differentiating between these two pathologies. In this work, hAGP was isolated by immunoaffinity chromatography (IAC) from serum samples of healthy individuals and from those suffering chronic pancreatitis and different stages of pancreatic cancer, respectively. After de-N-glycosylation, relative quantitation of the hAGP glycans was carried out using stable isotope labeling and μZIC-HILIC-ESI-MS analysis. First, protein denaturing conditions prior to PNGase F digestion were optimized to achieve quantitative digestion yields, and the reproducibility of the established methodology was evaluated with standard hAGP. Then, the proposed method was applied to the analysis of the clinical samples (control vs. pathological). Pancreatic cancer samples clearly showed an increase in the abundance of fucosylated glycans as the stage of the disease increases and this was unlike to samples from chronic pancreatitis. The results gained here indicate the mentioned glycan in h

  13. ROOTSTOCKS EFFECTS ON THE PHYSICOCHEMICAL CHARACTERISTICS OF BORDÔ, ISABEL AND IAC 138-22 MÁXIMO MUST AND WINE

    Directory of Open Access Journals (Sweden)

    MARLON JOCIMAR RODRIGUES DA SILVA

    2017-09-01

    Full Text Available ABSTRACT It has been demonstrated that rootstocks can influence grape characteristics, but there are few data in literature about the rootstocks influence in the wine characteristics, especially in wines elaborated with Vitis labrusca or hybrid grapes. This study evaluated the influence of ‘IAC 766’ and ‘106-8 Mgt’ rootstocks on the physicochemical characteristics of ‘Bordô’, ‘Isabel’ and ‘IAC 138-22 ‘Máximo’ musts and wines. The musts were evaluated for pH, soluble solids, total acidity and soluble solids/acidity ratio. The wines were evaluated for density, alcohol content; total, volatile and fixed acidity; pH, dry extract, reducing sugars, reduced dry extract, alcohol in weight/reduced dry extract; free and total sulfur dioxide; anthocyanins, polyphenols index (I 280; polyphenols and total flavonoids and antioxidant activity. The ‘Bordô’, ‘Isabel’ and IAC 138-22 ‘Máximo’ musts had low soluble solids for winemaking. The ‘106-8 Mgt’ rootstock promoted higher dry extract content and reduced dry extract in Bordô wine, and lower total and fixed acidity in IAC 138-22 Máximo wine. In Isabel wine, higher pH was promoted by the ‘IAC 766’ rootstock. Aside from low total acidity of the Bordô wine, all the physicochemical characteristics of the wines studied are in accordance with Brazilian law. There was no effect of rootstocks in the phenolics content and antioxidant activity of wines.

  14. Survey of aflatoxins in retail samples of whole and ground black and white peppercorns.

    Science.gov (United States)

    Adzahan, N; Jalili, M; Jinap, S

    2009-01-01

    A total of 126 local and imported samples of commercial white and black pepper in Malaysia were analysed for aflatoxins B1, B2, G1 and G2 (AFB1, AFB2, AFG1, AFG2) content using high-performance liquid chromatography (HPLC) with a fluorescence detector (FD). An acetonitrile-methanol-water (17 : 29 : 54; v/v) mixture was used as a mobile phase and clean-up was using an immunoaffinity column (IAC). Seventy out of 126 (55.5%) samples were contaminated with total aflatoxins, although only low levels of aflatoxins were found ranging from 0.1 to 4.9 ng g(-1). Aflatoxin B1 showed the highest incidence of contamination and was found in all contaminated samples. There was a significant difference between type of samples and different brands (p < 0.05). The results showed black peppers were more contaminated than white peppers.

  15. Development of microparticles for oral administration of the non-conventional radical scavenger IAC and testing in an inflammatory rat model.

    Science.gov (United States)

    Passerini, Nadia; Albertini, Beatrice; Sabatino, Marcello Di; Corace, Giuseppe; Luppi, Barbara; Canistro, Donatella; Vivarelli, Fabio; Cirillo, Silvia; Soleti, Antonio; Merizzi, Giulia; Paolini, Moreno

    2016-10-15

    The bis (1-hydroxy-2,2,6,6-tetramethyl-4-piperidinyl)-decandioate (IAC), is an innovative non- radical scavenger used with success in numerous disease models such as inflammation, neurological disorders, hepatitis and diabetes. The pharmacological treatments have been performed by the intraperitoneal route of administration, representing to date, the main limit for the drug use. The aim of this study was to develop a delivery system that allows the oral administration of IAC while maintaining its therapeutic efficacy. Solid Lipid Microparticles (SLMs) containing a theoretical 18% (w/w) of IAC have been produced by the spray congealing technology; three formulations have been tested (A, B and C) using different low melting point carriers (stearic acid, Compritol(®) HD5ATO and carnauba wax) alone or in combination. All IAC loaded SLMs exhibited a spherical shape, encapsulation efficiency higher than 94% and particle size suitable for the oral route. Administered per os at different dosages in an inflammation rat model, all SLMs demonstrated their efficacy in reducing oedema and alleviating pain, compared to the gold standards Indomethacin and Paracetamol. These results suggested that the SLMs are an efficacious delivery system for the oral administration of IAC, potentially useful for the treatment of others diseases related to an over production of free radicals. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Monitoramento das propriedades térmicas das borrachas naturais de novos clones: IAC 301 e IAC 303

    Directory of Open Access Journals (Sweden)

    Rogério M. B. Moreno

    2013-01-01

    Full Text Available A borracha natural (BN de três clones de seringueira [Hevea brasiliensis (Willd. exAdr. de Juss. Muell.-Arg.] de um período de sete meses foi obtida por coagulação do látex com solução de ácido acético a 10% e seca a 65°C. As curvas TG-DTG foram utilizadas para monitorar as propriedades térmicas da BN. Os resultados indicaram pequenas variações entre clones e coletas, exceto no valor de Tf-T0, indicando que o clone IAC 301 sofre degradação mais rápida durante o processo termo degradação da BN seca. Não houve diferenças significativas nos valores de Tg entre clones e coletas.

  17. Optimization of antibody immobilization for on-line or off-line immunoaffinity chromatography

    DEFF Research Database (Denmark)

    Beyer, Natascha Helena; Schou, Christian; Højrup, Peter

    2009-01-01

    -POROS. Protein G-based matrices are very stable showing essentially no decline in performance after 50 application-wash-elution-reequilibration cycles and being easily prepared within 2-3 h of working time with a typical antibody coupling yield of above 80%. In off-line applications where constant flow....... A systematic study was conducted to determine the most versatile antibody immobilization method for use in on-line and off-line IA chromatography applications using commonly accessible immobilization methods. Four chemistries were examined using polyclonal and monoclonal antibodies and antibody fragments. We...

  18. Leaf anatomy of cassava (Manihot esculenta Crantz. cv. IAC-12 after herbicides application to control weeds in Minas Gerais, Brazil

    Directory of Open Access Journals (Sweden)

    Daniel Valadão Silva

    2017-07-01

    Full Text Available Micro-morphological changes precede the appearance of visible damage after herbicide application and are essential in providing data for the safe recommendation in chemical management of weeds. Therefore, the aim of this research was to verify the anatomical changes of leaf tissue caused by application of herbicides in cassava (Manihot esculenta Crantz. cv. IAC-12. A greenhouse experiment was conducted with post-emergence herbicides treatments as follows: nicossulfuron (60 g a.i ha-1, fluazifop (250 g a.i ha-1, fomesafem (250 g a.i ha-1, metribuzin (480 g a.i ha-1, oxyfluorfen (720 g a.i ha-1 and the mixture fluazifop + fomesafen (200 + 250 g a.i ha-1, and an untreated control, respectively. The results obtained have allowed to affirm the cassava plants (cultivar IAC-12, exhibited changes in leaf anatomy in response to herbicide application even on cassava leaves without no visual toxicity symptoms. The products caused alterations both in tissue thickness as in tissue proportion in the leaf blade. For the fluazifop, a eudicotyledonous selective herbicide, changes were observed in tissue thickness and proportion of leaf blade, even without any visual toxicity detected. Cassava plants (IAC-12, showed structural changes in leaf anatomy in response to application of herbicides. The leaf anatomy of cassava cv. IAC-12, can be used to indicate the herbicide effect on cassava (Manihot esculenta Crantz.cv. IAC-12 plants.

  19. Radioimmunoassay of glandular kallikrein in human plasma after partial purification by immunoaffinity column

    International Nuclear Information System (INIS)

    Nishimura, Kazutaka; Inoue, Yoshikazu; Kokubu, Tatsuo

    1987-01-01

    Glandular kallikrein in human plasma was partially purified by immunoaffinity column and was measured by a radioimmunoassay (RIA). Plasma was diluted with an equal volume of 10 mmol/l sodium phosphate buffer, pH 7.4, containing 0.9% NaCl (PBS) and was applied to an immunoaffinity column from which glandular kallikrein was eluted with 3 mol/l NaSCN (20 ml). The enzymic fraction was concentrated with an Amicon PM 10 filter and dialyzed against PBS. The final recovery of the enzyme was 51.6 ± 1.6%, determined by using [ 125 I]kallikrein. The usable range of the standard curve covered 2.5-100 ng/tube. The coefficient of variation within the series was 5.9%, and the coefficient of variation between the series was 7.6%. In healthy controls, the plasma content of glandular kallikrein was 1.36 ± 0.39 ng/ml. In patients with acute pancreatitis, the plasma concentration was 8.02 ± 6.15 ng/ml, significantly different from the control group. (Auth.)

  20. ROOTSTOCKS EFFECTS ON THE PHYSICOCHEMICAL CHARACTERISTICS OF BORDÔ, ISABEL AND IAC 138-22 MÁXIMO MUST AND WINE

    OpenAIRE

    MARLON JOCIMAR RODRIGUES DA SILVA; LUCIANA TREVISAN BRUNELLI; MARA FERNANDES MOURA; JOSÉ LUIZ HERNANDES; SARITA LEONEL; MARCO ANTONIO TECCHIO

    2017-01-01

    ABSTRACT It has been demonstrated that rootstocks can influence grape characteristics, but there are few data in literature about the rootstocks influence in the wine characteristics, especially in wines elaborated with Vitis labrusca or hybrid grapes. This study evaluated the influence of ‘IAC 766’ and ‘106-8 Mgt’ rootstocks on the physicochemical characteristics of ‘Bordô’, ‘Isabel’ and ‘IAC 138-22 ‘Máximo’ musts and wines. The musts were evaluated for pH, soluble solids, total acidity and...

  1. Radiosurgery for Para-IAC Meningiomas: The Effect of Radiation Dose to the Cochlea on Hearing Outcome

    International Nuclear Information System (INIS)

    Kim, Young-Hoon; Kim, Dong Gyu; Han, Jung Ho; Chung, Hyun-Tai; Kim, In Kyung; Song, Sang Woo; Park, Jeong-Hoon; Kim, Jin Wook; Kim, Yong Hwy; Park, Chul-Kee; Kim, Chae-Yong; Paek, Sun Ha; Jung, Hee-Won

    2012-01-01

    Purpose: This study was performed to assess the radiosurgical results of meningiomas extending into the internal acoustic canal (para-IAC meningiomas), with a particular focus on the effect of radiation dose to the cochlea on hearing outcome. Methods and Materials: A total of 50 patients who underwent radiosurgery for para-IAC meningiomas between 1998 and 2009, which were followed for 2 years, were enrolled. The mean age was 55.8 years (range, 15–75). The mean tumor volume was 6.1 cm 3 (range, 1.0–19.0), the mean tumor length in the IAC was 6.9 mm (range, 1.3–13.3), and the mean prescribed marginal dose was 13.1 Gy (range, 10–15) at an isodose line of 50%. The mean follow-up duration was 46 months (range, 24–122). Results: Eight (16.0%) patients had nonserviceable hearing at the time of surgery. At the last follow-up, the tumor control rate was 94%; unchanged in 17 patients, decreased in 30 patients, and increased in 3 patients. Among 42 patients with serviceable hearing at the time of radiosurgery, it was preserved in 41 (97.6%) patients at the last follow-up. The maximal and mean radiation doses to the cochleae of these 41 patients were 5.8 Gy ± 0.3 (range, 3.1–11.5) and 4.3 Gy ± 0.2 (range, 2.2–7.5), respectively. The maximal dose to the cochlea of the patient who lost hearing after radiosurgery was 4.7 Gy. Conclusions: The radiation dose to the cochlea may have the minimal toxic effect on the hearing outcome in patients who undergo radiosurgery for para-IAC meningiomas.

  2. Best practices in energy management: Experience with IAC assessments in the metals fabrication industry

    International Nuclear Information System (INIS)

    Clark, W.J.; Birkmire, L.K.

    1999-01-01

    The Industrial Technology and Energy Management (ITEM) division of the University City Science Center played a managerial role in founding and establishing the Energy Analysis and Diagnostic Center (EADC) program, now known as the Industrial Assessment Center (IAC) program. ITEM is responsible for the field management of 15 IACs in the western US. This DOE funded program utilizes teams of engineering faculty and students to conduct assessments of small to medium-size plants to identify cost savings by conserving energy, minimizing waste, and improving productivity. These assessments are provided at no direct cost to participating manufacturers, who are under no obligation to act on any recommendations. Centers managed by ITEM have conducted assessments in more than 700 plants in the metals fabrication industry (SIC 34). Recommendations made have the potential to reduce energy costs by about 10% on average. The average metals fabrication plant served achieved a 5.7% reduction in annual energy costs. These cost savings are accompanied by a reduction in energy usage of about 1.2 x 10 12 Btu/yr. Another benefit of the program is that it provides hands-on industrial experience and energy efficiency training for engineering students who will take these skills into industry. Since the program began more than 20 years ago, IACs have served less than 2% of the plants in this industry. To provide an effective means for plant managers to access and utilize the knowledge gained over the years ITEM has summarized recommendations that identify specific actions that plant management can take to save money

  3. Analysis of clinical characteristics and treatment of immunoglobulin G4-associated cholangitis: A retrospective cohort study of 39 IAC patients.

    Science.gov (United States)

    Xiao, Jianchun; Xu, Peiran; Li, Binglu; Hong, Tao; Liu, Wei; He, Xiaodong; Zheng, Chaoji; Zhao, Yupei

    2018-02-01

    Immunoglobulin (Ig)G4-associated cholangitis (IAC) is one of the common organ manifestations of IgG4-related systemic disease (ISD). IAC and autoimmune pancreatitis (AIP) may mimic sclerosing cholangitis, cholangiocarcinoma, or pancreatic carcinoma. Diagnosis is based on a combination of clinical, biochemical, radiological, and histological findings.To study the clinical presentation of and treatment strategy for IAC, we reviewed clinical, serologic, and imaging characteristics, as well as treatment response, in 39 patients with IAC. The majority of patients were men (82%). Clinical features on presentation included obstructive jaundice in 26 patients (67%) and abdominal pain in 20 (51%). Positive IgG4 immunostaining was seen in 27 patients. The median serum IgG4 level before treatment was 769.4 mg/dL (range, 309.1-1229.7 mg/dL). After the steroid therapy, the median serum IgG4 level in 23 patients was 247.0 mg/dL (range, 139.0-355.0 mg/dL). Cholangiograms were available in 36 (92%) patients. Stenosis of the lower part of the common bile duct was found in 26 of 39 patients. Stenosis was diffusely distributed in the intra- and extrahepatic bile ducts in 14 of 39 patients. Additionally, strictures of the bile duct were detected in the hilar hepatic lesions in 27 of 39 patients. AIP was the most frequent comorbidity (35/39 in this study) of IAC. Other affected organs included eyes (n = 6), salivary glands (sialadenitis, n = 10), lymph nodes (mediastinal and axillary, n = 3), kidneys (n = 2), and the retroperitoneum (retroperitoneal fibrosis, n = 2).Regarding treatment, 29 patients were treated with steroids, of whom one underwent pancreatoduodenectomy, and one underwent choledochojejunostomy. Eight patients were treated with biliary stents. The remaining 19 patients took prednisolone alone. Eight patients achieved spontaneous resolution. Four patients with suspected pancreatic cancer or cholangiocarcinoma underwent surgery, including 2

  4. MELHORAMENTO GENÉTICO DO TRIGO: XXXII. AVALIAÇÃO DE NOVOS GENÓTIPOS DERIVADOS DO 'IAC 24' QUANTO ÀS CARACTERÍSTICAS AGRONÔMICAS E À QUALIDADE TECNOLÓGICA

    Directory of Open Access Journals (Sweden)

    FELÍCIO JOÃO CARLOS

    1998-01-01

    Full Text Available Avaliaram-se 29 genótipos de trigo provenientes de cruzamentos entre o cultivar IAC 24 e fontes comprovadas de resistência a Puccinia recondita e características específicas para panificação, mais o cultivar IAC 24 (controle, mediante experimentos semeados em diferentes regiões tritícolas paulistas no período 1993-95. Analisaram-se as características seguintes: produtividade de grãos, resistência à ferrugem-da-folha, à tolerância ao alumínio tóxico e às qualidades industriais para pão. Considerando a produtividade, destacou-se, no Vale do Paranapanema, o genótipo no 24 (CM H. 74A-630/SX//CNO79/3/IAC 24; na região de Capão Bonito, o no 26 (Yaco "S"/IAC -24 e, em Mococa, com irrigação por aspersão, o no 23 (CM 6530/IAC-24. A resistência ao agente causal da ferrugem-da-folha foi transferida para os genótipos por meio dos cruzamentos envolvendo Yaco "S" e Agent/6*SKA//AGA/4/TI71. Seis genótipos entre os avaliados revelaram-se muito sensíveis ao Al3+ Os trigos duros apresentaram maior rendimento de extração de farinha, comparados aos moles. Considerando os diferentes parâmetros avaliados para qualidade tecnológica, destacaram-se os genótipos no 16 (IAS58/IAS55//ALD/3/IAC5/4/ALD/IAS58/8.1034.A//ALD/5/CNR/6/BUC"S"/7/IAC24 e no 12 (MRNG/4/NAD/FOR//PCN/3/BLT/MES/5/PAT2195*2/ZP"S"/6/ALD/EMU//CHAT/7/VEE/8/IAC24, com base no estudo da divergência genética por componentes principais.

  5. Propriedades físico-químicas do amido de aveia da variedade brasileira IAC 7 Physicochemical properties of IAC 7 oat starch from Brazilian cultivars

    Directory of Open Access Journals (Sweden)

    Melicia Cintia Galdeano

    2009-12-01

    Full Text Available Este estudo caracterizou o amido de aveia da variedade IAC-7 quanto às suas características químicas, reológicas, funcionais e térmicas. O amido de aveia apresentou 1,36% de lipídios, 32,23% de amilose e baixa capacidade retrogradante (9,19% após 30 dias de armazenagem. Embora o amido de aveia tenha apresentado alto teor de amilose, sua baixa retrogradação pode ser devida à presença dos lipídios que, por impedimento estérico, dificultariam a reaproximação das cadeias poliméricas. O comportamento reológico das pastas de amido de aveia foi caracterizado como sendo pseudoplático. A baixa temperatura de gelatinização (64,71 °C do amido de aveia também pode estar relacionada ao maior teor de lipídio deste amido.This study characterized the chemical, rheological, functional and thermal properties of oat starch of IAC-7 variety. The oat starch showed 1.36% of lipids, 32.23% of amylose and low retrogradation capacity (9.19% after 30 days of storage. Although the oat starch has presented high amylose content, its low retrogradation may be due to the presence of lipids that by steric impediment could make it difficult for the polymeric chains to approach. The rheological behavior of oat starch was characterized as pseudoplastic. The low gelatinization temperature (64.71 °C of the starch may be related to its higher lipid content.

  6. A proteomics method using immunoaffinity fluorogenic derivatization-liquid chromatography/tandem mass spectrometry (FD-LC-MS/MS) to identify a set of interacting proteins.

    Science.gov (United States)

    Nakata, Katsunori; Saitoh, Ryoichi; Ishigai, Masaki; Imai, Kazuhiro

    2018-02-01

    Biological functions in organisms are usually controlled by a set of interacting proteins, and identifying the proteins that interact is useful for understanding the mechanism of the functions. Immunoprecipitation is a method that utilizes the affinity of an antibody to isolate and identify the proteins that have interacted in a biological sample. In this study, the FD-LC-MS/MS method, which involves fluorogenic derivatization followed by separation and quantification by HPLC and finally identification of proteins by HPLC-tandem mass spectrometry, was used to identify proteins in immunoprecipitated samples, using heat shock protein 90 (HSP90) as a model of an interacting protein in HepaRG cells. As a result, HSC70 protein, which was known to form a complex with HSP90, was isolated, together with three different types of HSP90-beta. The results demonstrated that the proposed immunoaffinity-FD-LC-MS/MS method could be useful for simultaneously detecting and identifying the proteins that interact with a certain protein. Copyright © 2017 John Wiley & Sons, Ltd.

  7. Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Neng-Zhi [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Liu, Ping [School of Pharmaceutical Science, Guangxi Medical University, Nanning, Guangxi 530021 (China); Su, Xiao-Chuan; Liao, Yan-Hua; Lei, Ning-Sheng [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Liang, Yong-Hong [School of Pharmaceutical Science, Guangxi Medical University, Nanning, Guangxi 530021 (China); Zhou, Shao-Huan; Lin, Wen-Si; Chen, Jie [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China); Feng, Yu-Qi [Key Laboratory of Analytical Chemistry for Biology and Medicine, Ministry of Education, Department of Chemistry, Wuhan University, Wuhan 430072 (China); Tang, Yang, E-mail: tycarson2@163.com [Guangxi Zhuang Autonomous Region Center for Disease Prevention and Control, Nanning, Guangxi 530028 (China)

    2017-06-01

    Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B{sub 1}, B{sub 2}, G{sub 1}, and G{sub 2}) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were

  8. Aflatoxins and ochratoxin a reduction in black and white pepper by gamma radiation

    International Nuclear Information System (INIS)

    Jalili, M.; Jinap, S.; Noranizan, M.A.

    2012-01-01

    Irradiation is an important means of decontamination of food commodities, especially spices. The aim of the current study was to investigate the efficacy of gamma radiation ( 60 Co) for decontaminating ochratoxin A (OTA) and aflatoxins B 1 (AFB 1 ), B 2 (AFB 2 ), G 1 (AFG 1 ) and G 2 (AFG 2 ) residues in artificially contaminated black and white pepper samples. The moisture content of the pepper samples was set at 12% or 18%, and the applied gamma dose ranged from 5 to 30 kGy. Mycotoxin levels were determined by high-performance liquid chromatography (HPLC) after immunoaffinity column (IAC) chromatography. Both the gamma irradiation dose and moisture content showed significant effects (P<0.05) on mycotoxin reduction. The maximum toxin reductions, found at 18% moisture content and 30 kGy, were 55.2%, 50.6%, 39.2%, 47.7% and 42.9% for OTA, AFB1, AFB2, AFG1 and AFG2, respectively. - Highlights: ► The effect of gamma ray on the reduction of AFs and OTA in pepper was investigated. ► The gamma dose and moisture showed significant effects on mycotoxin reduction. ► The maximum reduction was found at 18% moisture content and 30 kGy gamma ray. ► The method, even at 30 kGy and 18% moisture, failed to destroy total of mycotoxins.

  9. Purification of nitrate reductase from Nicotiana plumbaginifolia by affinity chromatography using 5'AMP-sepharose and monoclonal antibodies.

    Science.gov (United States)

    Moureaux, T; Leydecker, M T; Meyer, C

    1989-02-15

    Nitrate reductase was purified from leaves of Nicotiana plumbaginifolia using either 5'AMP-Sepharose chromatography or two steps of immunoaffinity chromatography involving monoclonal antibodies directed against nitrate reductase from maize and against ribulose-1,5-bisphosphate carboxylase from N. plumbaginifolia. Nitrate reductase obtained by the first method was purified 1000-fold to a specific activity of 9 units/mg protein. The second method produced an homogenous enzyme, purified 21,000-fold to a specific activity of 80 units/mg protein. SDS/PAGE of nitrate reductase always resulted in two bands of 107 and 99.5 kDa. The 107-kDa band was the nitrate reductase subunit of N. plumbaginifolia; the smaller one of 99.5 kDa is thought, as commonly reported, to result from proteolysis of the larger protein. The molecular mass of 107 kDa is close to the values calculated from the coding sequences of the two nitrate reductase genes recently cloned from tobacco (Nicotiana tabacum cv Xanthi).

  10. Microchip Immunoaffinity Electrophoresis of Antibody-Thymidine Kinase 1 Complex

    Science.gov (United States)

    Pagaduan, Jayson V.; Ramsden, Madison; O’Neill, Kim; Woolley, Adam T.

    2015-01-01

    Thymidine kinase-1 (TK1) is an important cancer biomarker whose serum levels are elevated in early cancer development. We developed a microchip electrophoresis immunoaffinity assay to measure recombinant purified TK1 (pTK1) using an antibody that binds to human TK1. We fabricated poly(methyl methacrylate) microfluidic devices to test the feasibility of detecting antibody (Ab)-pTK1 immune complexes as a step towards TK1 analysis in clinical serum samples. We were able to separate immune complexes from unbound antibodies using 0.5X phosphate buffer saline (pH 7.4) containing 0.01% Tween-20, with 1% w/v methylcellulose that acts as a dynamic surface coating and sieving matrix. Separation of the antibody and Ab-pTK1 complex was observed within a 5 mm effective separation length. This method of detecting pTK1 is easy to perform, requires only a 10 μL sample volume, and takes just 1 minute for separation. PMID:25486911

  11. Long-Term Occurrence of Deoxynivalenol in Feed and Feed Raw Materials with a Special Focus on South Korea

    Directory of Open Access Journals (Sweden)

    Juhee Park

    2018-03-01

    Full Text Available The Fusarium fungi produce toxic substances called mycotoxins, which can cause disease and harmful effects in grains, livestock, and humans. Deoxynivalenol (DON, also known as vomitoxin, is one of the Fusarium mycotoxins that is known to cause vomiting in livestock. This study shows the occurrence of deoxynivalenol in feedstuffs (compound feed and feed ingredients between 2009 and 2016 in South Korea. A total of 653 domestic samples were collected at five time points, including 494 compound feed samples and 159 feed ingredient samples. DON contamination levels were analyzed using high-performance liquid chromatography (HPLC with pretreatment using an immunoaffinity column (IAC. The limit of detection (LOD and the limit of quantification (LOQ were estimated at 1–10 µg/kg and 3–35 µg/kg, respectively. Two compound feeds (two gestating sow feed samples out of 160 pig feed samples exceeded the European Commission (EC guidance value, while no feed ingredient samples exceeded the EC or South Korean guidance values. There were statistically significant differences in the mean contamination levels of compound feed and feed ingredients that indicated a decreasing trend over time.

  12. Low-cost humic acid-bonded silica as an effective solid-phase extraction sorbent for convenient determination of aflatoxins in edible oils.

    Science.gov (United States)

    Zhou, Neng-Zhi; Liu, Ping; Su, Xiao-Chuan; Liao, Yan-Hua; Lei, Ning-Sheng; Liang, Yong-Hong; Zhou, Shao-Huan; Lin, Wen-Si; Chen, Jie; Feng, Yu-Qi; Tang, Yang

    2017-06-01

    Aflatoxins (AFs) are highly toxic, mutagenic, carcinogenic, and teratogenic secondary metabolites produced by the toxigenic fungi Aspergillus flavus and Aspergillus parasiticus. AFs tend to contaminate a wide range of foods which is a serious and recurring food safety problem worldwide. Currently, immunoaffinity chromatography (IAC) has become the most conventional sample clean-up method for determining AFs in foodstuffs. However, IAC method is limited in the large-scale food analysis because it requires the use of expensive disposable cartridges and the IA procedure is time-consuming. Herein, to achieve the cost-effective determination of AFs in edible oils, we developed a promising solid-phase extraction (SPE) method based on commercially available humic acid-bonded silica (HAS) sorbent, followed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS) analysis. In HAS-SPE, AFs can be captured by the HAS sorbent with both hydrophobic and hydrophilic interactions, whereas the oil matrix was captured only with the hydrophobic interactions. The oil matrix can be sufficiently washed off with isopropanol, while the AFs were still retained on the SPE packing, thus achieving selective extraction of AFs and clean-up of oil matrices. Under the optimal conditions of HAS-SPE, satisfactory recoveries ranging from 82% to 106% for four AFs (B 1 , B 2 , G 1 , and G 2 ) were achieved in various oil matrices, containing blended oil, tea oil, rapeseed oil, peanut oil, sunflower seed oil, corn oil, blended olive oil, rice oil, soybean oil, and sesame oil. Only minor matrix effects ranging from 99% to 105% for four AFs were observed. Moreover, the LODs of AFs between 0.012 and 0.035 μg/kg completely meet the regulatory levels fixed by the EU, China or other countries. The methodology was further validated for assaying the naturally contaminated peanut oils, and consistent results between the HAS-SPE and the referenced IAC were obtained. In

  13. Isolation of melatonin by immunoaffinity chromatography

    Czech Academy of Sciences Publication Activity Database

    Rolčík, Jakub; Lenobel, René; Siglerová, Věra; Strnad, Miroslav

    2002-01-01

    Roč. 25, č. 1 (2002), s. 9-15 ISSN 0378-4347 R&D Projects: GA MŠk OC 844.10; GA ČR GA301/02/0475 Institutional research plan: CEZ:AV0Z5038910 Keywords : Melatonin Subject RIV: CE - Biochemistry Impact factor: 1.913, year: 2002

  14. Centrifugal precipitation chromatography

    Science.gov (United States)

    Ito, Yoichiro; Lin, Qi

    2009-01-01

    Centrifugal precipitation chromatography separates analytes according their solubility in ammonium sulfate (AS) solution and other precipitants. The separation column is made from a pair of long spiral channels partitioned with a semipermeable membrane. In a typical separation, concentrated ammonium sulfate is eluted through one channel while water is eluted through the other channel in the opposite direction. The countercurrent process forms an exponential AS concentration gradient through the water channel. Consequently, protein samples injected into the water channel is subjected to a steadily increasing AS concentration and at the critical AS concentration they are precipitated and deposited in the channel bed by the centrifugal force. Then the chromatographic separation is started by gradually reducing the AS concentration in the AS channel which lowers the AS gradient concentration in the water channel. This results in dissolution of deposited proteins which are again precipitated at an advanced critical point as they move through the channel. Consequently, proteins repeat precipitation and dissolution through a long channel and finally eluted out from the column in the order of their solubility in the AS solution. The present method has been successfully applied to a number of analytes including human serum proteins, recombinant ketosteroid isomerase, carotenoid cleavage enzymes, plasmid DNA, polysaccharide, polymerized pigments, PEG-protein conjugates, etc. The method is capable to single out the target species of proteins by affinity ligand or immunoaffinity separation. PMID:19541553

  15. SELECTIVE INTRA-ARTERIAL CHEMOTHERAPY (IAC IN TREATMENT AT CHILDREN WITH THE INTRAOCULAR RETYNOBLASTOMA

    Directory of Open Access Journals (Sweden)

    I. V. Pogrebnyakov

    2018-01-01

    Full Text Available Treatment of intraocular retinoblastoma is challenging. It requires a multidisciplinary personalized approach that includes focal treatments, chemotherapy, surgery and radiotherapy. Today, the focus of therapy has shifted to eye preservation with the major aim to save the child’s life and to preserve the eyeball as a functioning organ of vision with minimal complications. One of the most promising therapy approaches is selective intra-arterial chemotherapy (IAC, by which a cytostatic agent is given directly into the eye. This treatment modality has been shown to provide survival benefit and improvement of quality of life, reducing toxicity and minimizing side effects.

  16. Arquitetura do sistema radicular do porta-enxerto de videira 'IAC 766' na época de transplante do viveiro para o campo Root architecture of IAC 766 grapevine rootstock in the transplanting from the nursery to the field

    Directory of Open Access Journals (Sweden)

    Ricardo Sfeir de Aguiar

    2006-12-01

    Full Text Available Na propagação de porta-enxertos de videira por estaquia em recipientes para posterior transplante ao campo, é importante evitar danos ao sistema radicular. O objetivo do trabalho foi determinar, por meio da avaliação da arquitetura do sistema radicular, a melhor fase de desenvolvimento da muda para o transplante, ao campo, do porta-enxerto de videira 'IAC 766' Campinas, em Marialva - PR. As plantas foram avaliadas aos 60; 90; 120; 150 e 180 dias após a estaquia lenhosa em substratos contidos em sacos plásticos de 20cm de largura por 30cm de altura. As raízes foram expostas e fotografadas, avaliando-se comprimento e área do sistema radicular pelo programa SIARCS 3.0. Foi utilizado também um diagrama de arquitetura radicular, atribuindo-se notas à conformação do sistema radicular e foi contado o número de raízes enoveladas. O delineamento experimental utilizado foi o de blocos inteiramente ao acaso, com cinco tratamentos e cinco repetições, com 10 plantas por parcela. Os dados foram submetidos à análise de regressão polinomial. Todas as características, com exceção das notas da arquitetura do sistema radicular, ajustaram-se ao modelo de regressão linear crescente. A melhor fase para o transplante da muda do porta-enxerto 'IAC 766' para o campo é aos 90 dias após a estaquia.In grapevine propagation with cuttings in containers it is important to avoid damages to root system during transplanting to the field. The aim of this research was to determine, by means of root system evaluation, the best period to transplant 'IAC 766' (Campinas rootstock. The trial was set up in July 2004 in Marialva County (PR. The plants were evaluated 60, 90, 120, 150 and 180 days after the establishment of woody cutting in plastic bags of 20cm wide and 30cm high. The roots were exposed and pictures were taken in lateral and top positions and were evaluated by SIARCS 3.0 software, with determination of the area and the length of the root system

  17. ASSOCIAÇÃO ENTRE O ÍNDICE DE ADIPOSIDADE CORPORAL (IAC E ÍNDICE DE MASSA CORPORAL (IMC EM MULHERES PRATICANTES DE TREINAMENTO RESISTIDO

    Directory of Open Access Journals (Sweden)

    William Cordeiro de Souza

    2014-04-01

    Full Text Available O presente estudo buscou como objetivo realizar uma relação entre o índice de adiposidade corporal (IAC e índice de massa corporal (IMC em mulheres praticantes de treinamento resistido. A mostra foi composta por 14 mulheres (idade: 27 ± 3.96 anos praticantes de treinamento resistido (3 a 5 dias por semana. Foram avaliados o peso e a estatura para obtenção de IMC e circunferência do quadril (CQ na determinação do índice de adiposidade corporal. Na análise dos dados foi utilizada à estatística descritiva: Média, desvio padrão (dp, frequência percentual (% e o fator de correlação de Pearson (r com nível de significância de 0,05. Nos resultados obtidos observou-se que no IMC todas as avaliadas estão dentro dos padrões estabelecidos (eutroficas. Com relação ao IAC, 28.57% (n=4 das mulheres avaliadas estão dentro do padrão “Ideal”, 42.87% (n=6 com seu percentual “Moderado” e 28.57% (n= 4 com “Excesso de gordura”. Quanto à circunferência do quadril foi verificado que as todas as avaliadas (n=14 estão com dentro dos padrões recomendo. Não foram encontradas correlações entre IMC e IAC (r =0,392 e p =0,164, nem entre IMC e CQ (r =0,272 e p =0,345. Ao finalizar o estudo foi verificado que não houve diferenças significativas entre IMC e IAC; nem para o IMC com a CQ.

  18. Development of a Positron Source for JLab at the IAC

    Energy Technology Data Exchange (ETDEWEB)

    Forest, Tony [Idaho State Univ., Pocatello, ID (United States)

    2013-10-12

    We report on the research performed towards the development of a positron sour for Jefferson Lab's (JLab) Continuous Electron Beam Accelerator Facility (CEBAF) in Newport News, VA. The first year of work was used to benchmark the predictions of our current simulation with positron production efficiency measurements at the IAC. The second year used the benchmarked simulation to design a beam line configuration which optimized positron production efficiency while minimizing radioactive waste as well as design and construct a positron converter target. The final year quantified the performance of the positron source. This joint research and development project brought together the experiences of both electron accelerator facilities. Our intention is to use the project as a spring board towards developing a program of accelerator based research and education which will train students to meet the needs of both facilities as well as provide a pool of trained scientists.

  19. Comparison of High Performance Liquid Chromatography with Fluorescence Detector and with Tandem Mass Spectrometry methods for detection and quantification of Ochratoxin A in green and roasted coffee beans

    Directory of Open Access Journals (Sweden)

    Raquel Duarte da Costa Cunha Bandeira

    2013-12-01

    Full Text Available Two analytical methods for the determination and confirmation of ochratoxin A (OTA in green and roasted coffee samples were compared. Sample extraction and clean-up were based on liquid-liquid phase extraction and immunoaffinity column. The detection of OTA was carried out with the high performance liquid chromatography (HPLC combined either with fluorescence detection (FLD, or positive electrospray ionization (ESI+ coupled with tandem mass spectrometry (MS-MS. The results obtained with the LC-ESI-MS/MS were specific and more sensitive, with the advantages in terms of unambiguous analyte identification, when compared with the HPLC-FLD.

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

    Science.gov (United States)

    Hyung, Seok-Won; Piehowski, Paul D; Moore, Ronald J; Orton, Daniel J; Schepmoes, Athena A; Clauss, Therese R; Chu, Rosalie K; Fillmore, Thomas L; Brewer, Heather; Liu, Tao; Zhao, Rui; Smith, Richard D

    2014-11-01

    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 (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 maximizing 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 microscale 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 microscale column increased as flow rate decreased, and that our microdepletion was reproducible. In an initial application, a 600-μL sample of human cerebrospinal 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.

  1. Sistemas Correctores de Campo Para EL Telescopio Cassegrain IAC80

    Science.gov (United States)

    Galan, M. J.; Cobos, F. J.

    1987-05-01

    El proyecto de instrumentación de mayor importancia que ha tenido el Instituto de Astrofisica de Canarias en los últimos afios ha sido el diseflo y construcción del te1escopio IAC8O. Este requería del esfuerzo con junto en mec´nica, óptica y electrónica, lo que facilitó la estructuración y el crecimiento de los respectivos grupos de trabajo, que posteriormente se integraron en departamentos En su origen (1977), el telescopio IAC80 fue concebido como un sistema clásico tipo Cassegrain, con una razón focal F/i 1.3 para el sistema Casse grain y una razón focal F/20 para el sistema Coudé. Posteriormente, aunque se mantuvo la filosofia de que el sistema básico fuera el F/11.3, se consideró conveniente el diseño de secundarios para razones focales F/16 y F/32, y se eliminó el de F/20. Sin embargo, dada la importancia relativa que un foco estrictamente fotográfico tiene en un telescopio moderno, diseñado básicamente para fotometría fotoeléctrica y con un campo util mínimamente de 40 minutos de arco, se decídió Ilevar a cabo el diseño de un secundario F/8 con un sistema corrector de campo, pero que estuviera formado únicamente por lentes con superficies esféricas para que asl su construcción fuera posible en España ó en México. La creciente utilización de detectores bidimensionales para fines de investigación astron6mica y la viabilidad de que en un futuro cercano éstos tengan un área sensible cada vez mayor, hicieron atractiva la idea de tener diseñado un sistema corrector de campo para el foco primario (F/3), con un campo útil mínimo de un grado, y también con la limitante de que sus componentes tuvieron sólamente supérficies esféricas. Ambos diseños de los sis-temas correctores de campo se llevaron a cabo, en gran medida, como parte de un proyecto de colaboración e intercambio en el área de diseño y evaluación de sistemas ópticos.

  2. Comparison of two sample preparation procedures for HPLC determination of ochratoxin A

    Directory of Open Access Journals (Sweden)

    Vuković Gorica L.

    2009-01-01

    Full Text Available In preparation of samples for chromatographic determination of ochratoxin A, two types of columns were used for sample cleanup (SPE and immunoaffinity columns. The first method consisted of liquid-liquid extraction with a mixture of chloroform and phosphoric acid, followed by ion-exchange cleanup on Waters Oasis MAX columns. The sec­ond method consisted of extraction with a mixture of water and methanol, followed by LCTech OtaCLEAN immunoaf­finity column cleanup. Recoveries of the methods were determined at three levels in three repetitions for maize flour, and they were 84% (%RSD = 19.2 for the first method of sample preparation and 101% (%RSD = 2.2 for the second method. Values of LOQ for OTA were 0.25 and 1.00 μg/kg for the IAC and SPE clean-up procedures, respectively. Both methods comply with present regulations, but the MAX sample clean-up procedure should be used as an alternative, since the immunoaffinity column clean-up procedure is characterized by better reproducibility, accuracy, and efficiency.

  3. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa.

    Science.gov (United States)

    Liu, Xiaofei; Ying, Guangyao; Sun, Chaonan; Yang, Meihua; Zhang, Lei; Zhang, Shanshan; Xing, Xiaoyan; Li, Qian; Kong, Weijun

    2018-01-01

    The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD) after ultrasonication-assisted extraction, immunoaffinity column (IAC) clean-up and on-line post-column photochemical derivatization (PCD). Aflatoxins B 1 , B 2 , G 1 , G 2 were extracted from samples by using methanol/water (70:30, v/v ) with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0) to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity ( R > 0.999), sensitivity (limits of detection (LODs) and limits of quantitation (LOQs) of 0.15-0.65 and 0.53-2.18 μg/kg, respectively), precision (RSD sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B 1 (AFB 1 ) at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  4. Determination of ochratoxin A in wine by means of immunoaffinity and aminopropyl solid-phase column cleanup and fluorometric detection.

    Science.gov (United States)

    Longobardi, Francesco; Iacovelli, Vito; Catucci, Lucia; Panzarini, Giuseppe; Pascale, Michelangelo; Visconti, Angelo; Agostiano, Angela

    2013-02-27

    A new analytical method for the determination of ochratoxin A (OTA) in red wine has been developed by using a double-extract cleanup and a fluorometric measurement after spectral deconvolution. Wine samples were diluted with a solution containing 1% polyethylene glycol and 5% sodium hydrogencarbonate, filtered, and purified by immunoaffinity and aminopropyl solid-phase column. OTA contents in the purified extract were determined by a spectrofluorometer (excitation wavelength, 330 nm; emission wavelength, 470 nm) after deconvolution of fluorescence spectra. Average recoveries from wine samples spiked with OTA at levels ranging from 0.5 to 3.0 ng/mL were 94.5-105.4% with relative standard deviations (RSD) of <15% (n = 4). The limit of detection (LOD) was 0.2 ng/mL, and the total time of analysis was 30 min. The developed method was tested on 18 red wine samples (naturally contaminated and spiked with OTA at levels ranging from 0.4 to 3.0 ng/mL) and compared with AOAC Official Method 2001.01, based on immunoaffinity column cleanup and HPLC with fluorescence detector. A good correlation (r(2) = 0.9765) was observed between OTA levels obtained with the two methods, highlighting the reliability of the proposed method, the main advantage of which is the simple OTA determination by a benchtop fluorometer with evident reductions of cost and time of analysis.

  5. Results on the application of the methodology for power diagnoses Iac-DOE to Mexican companies; Resultados de la aplicacion de la metodologia de diagnosticos energeticos Iac-DOE a empresas mexicanas

    Energy Technology Data Exchange (ETDEWEB)

    Ambriz Garcia, Juan Jose [Universidad Autonoma de Mexico, Mexico, D.F. (Mexico)

    2001-07-01

    This work presents an analysis of the results of eight industrial power audits made in Mexico by a team of professors and students of the Universidad Autonoma Metropolitana-Ixtapalapa (UAM), following the methodology of the Centers of Industrial Consultant's office and Analyses and Power Diagnoses sponsored by the Office of Industrial Technologies of the Department of Energy of the United Studies (IAC-DOE Program). In these diagnosis studies, that could be classified as of fast execution, it was possible to find and to evaluate from 6 to 13 actions by company to increase their energy efficiency. This represents at the moment between 6 and 29% of the currently used energy, being the average 18.4%. The equivalent economic saving ascends to a value between 7 and 31% of the total paid, with an average value of 13.8%. Finally, the simple period of return for the saving recommendations is of 0.87 years, with an average number of 0.51 years for the actions focused to the saving of thermal energy and 1.52 years for the actions that improve the use of the electric energy. [Spanish] Este trabajo se presenta un analisis de los resultados de ocho auditorias energeticas industriales realizadas en Mexico por un equipo de profesores y estudiantes de la Universidad Autonoma Metropolitana-Iztapalapa (UAM), siguiendo la metodologia de los Centros de Asesoria Industrial y de Analisis y Diagnosticos Energeticos patrocinados por la Oficina de Tecnologias Industriales del Departamento de Energia de los Estudios Unidos (Programa IAC-DOE). En estos estudios de diagnostico, que podrian ser clasificados como de rapida ejecucion, fue posible encontrar y evaluar de 6 a 13 acciones por empresa para incrementar su eficiencia energetica. Esto representa entre 6 y 29% de la energia empleada actualmente, siendo el promedio del 18.4%. El ahorro economico equivalente asciende a un valor entre 7 y 31% del total pagado, con un valor promedio de 13.8%. Finalmente, e periodo simple de retorno para

  6. Maturação e produção de sementes de gergelim cultivar IAC-China

    Directory of Open Access Journals (Sweden)

    Lago Antonio Augusto do

    2001-01-01

    Full Text Available Este trabalho teve por objetivo avaliar o desenvolvimento e a qualidade fisiológica e física de sementes de gergelim (Sesamum indicum L. cultivar IAC-China, durante a fase de maturação. O estudo foi realizado por dois anos agrícolas consecutivos, em plantios tardios "das águas", em área homogênea do Instituto Agronômico, em Campinas, SP. As colheitas foram feitas a intervalos de três a sete dias até os 150 dias após emergência no campo em 1993/1994, e aos 144 dias em 1994/1995. Em cada colheita foram efetuadas as seguintes determinações: conteúdo de umidade das sementes e frutos, massa seca de mil sementes, produção por planta, e germinação até 18 meses de armazenamento em condições não controladas. Os mais altos valores de massa seca de mil sementes, as maiores produções e as menores perdas de sementes por degrana ocorreram aos 132 dias após emergência no ano agrícola 1993/1994, e aos 116 dias em 1994/1995. Nesses pontos ótimos de colheita, as sementes apresentaram graus de umidade inadequados à sua preservação; após apropriada secagem, exibiram altos índices de germinação aos zero, seis, doze e dezoito meses de armazenamento. Considerando-se os anos agrícolas, pode-se afirmar que o melhor período de colheita de gergelim da cultivar IAC-China está situado entre 116 e 132 dias após a emergência no campo.

  7. Analysis of Serum Total and Free PSA Using Immunoaffinity Depletion Coupled to SRM: Correlation with Clinical Immunoassay Tests

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Tao; Hossain, Mahmud; Schepmoes, Athena A.; Fillmore, Thomas L.; Sokoll, Lori J.; Kronewitter, Scott R.; Izmirlian, Grant; Shi, Tujin; Qian, Weijun; Leach, Robin; Thompson, Ian M.; Chan, Daniel W.; Smith, Richard D.; Kagan, Jacob; Srinivastava, Sudhir; Rodland, Karin D.; Camp, David G.

    2012-08-03

    Sandwich immunoassay is the standard technique used in clinical labs for quantifying protein biomarkers for disease detection, monitoring and therapeutic intervention. Albeit highly sensitive, the development of a specific immunoassay is rather time-consuming and associated with extremely high cost due to the requirement for paired immunoaffinity reagents of high specificity. Recently, mass spectrometry-based methods, specifically selected reaction monitoring mass spectrometry (SRM-MS), have been increasingly applied to measure low abundance biomarker candidates in tissue and biofluids, owing to high sensitivity and specificity, simplicity of assay configuration, and great multiplexing capability. In this study, we report for the first time the development of immunoaffinity depletion-based workflows and SRM-MS assays that enable sensitive and accurate quantification of total and free prostate-specific antigen (PSA) in serum without the requirement for specific PSA antibodies. With stable isotope dilution and external calibration, low ng/mL level detection of both total and free PSA was consistently achieved in both PSA-spiked female serum samples and actual patient serum samples. Moreover, comparison of the results obtained when SRM PSA assays and conventional immunoassays were applied to the same samples showed very good correlation (R2 values ranging from 0.90 to 0.99) in several independent clinical serum sample sets, including a set of 33 samples assayed in a blinded test. These results demonstrate that the workflows and SRM assays developed here provide an attractive alternative for reliably measuring total and free PSA in human blood. Furthermore, simultaneous measurement of free and total PSA and many other biomarkers can be performed in a single analysis using high-resolution liquid chromatographic separation coupled with SRM-MS.

  8. Fertilization with nitrogen and potassium in banana cultivars ‘Grand Naine’, ‘FHIA 17’ and ‘Nanicão IAC 2001’ cultivated in Ribeira Valley, São Paulo State, Brazil

    Directory of Open Access Journals (Sweden)

    Edson Shigueaki Nomura

    2017-08-01

    Full Text Available The ‘Grand Naine’ banana cultivar is grown around the world, but it is susceptible to black Sigatoka fungus. The ‘FHIA 17’ and ‘Nanicão IAC 2001’ cultivars have the potential to replace susceptible cultivars, but there is little information about their nitrogen and potassium nutritional requirements. This study aimed to identify the best fertilizer recommendation with N and K for banana cultivars ‘FHIA 17’, ‘Nanicão IAC 2001’, and ‘Grand Naine’. The applied fertilizer levels with N and K2O in two production cycles were as follows: NK0, without fertilization; NK1, 175 N and 285 kg K2O ha-1 year-1; NK2, 350 N and 570 kg K2O ha-1 year-1; and NK 3, 525 N and 855 kg K2O ha-1 year-1. It was concluded that the N and K fertilization levels influenced most of the phenological and production parameters of ‘Grand Naine’ and ‘Nanicão IAC 2001’. ‘Nanicão IAC 2001’ and ‘Grand Naine’ achieved maximum yield with an application of 525 kg N ha-1 year-1 and 855 kg K2O ha-1 year-1. The ‘FHIA 17’ cultivar showed a low response to nitrogen and potassium fertilization. Regardless of cultivars, to achieve maximum productivity (44.2 and 43.3 ton ha-1 year-1, an application at 150% and 124% of the fertilizer recommendation is required in the 1st and 2nd production cycles, respectively.

  9. Quantitation of antibodies to nucleoribonucleoprotein by ELISA : relation between antibody levels and disease activity in patients with connective tissue disease

    NARCIS (Netherlands)

    Houtman, PM; Kallenberg, CGM; Limburg, PC; Huitema, MG; van Rijswijk, MH; The, TH

    1985-01-01

    We describe a solid-phase enzyme-linked immunosorbent assay (ELISA) for quantitation of antibodies to nucleoribonucleoprotein (nRNP/Sm). nRNP/Sm was purified from rabbit thymus acetone powder by immunoaffinity chromatography and characterized by counterimmunoelectrophoresis (CIE) and immunoblotting

  10. On-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry using Fab´antibody fragments for the analysis of serum transthyretin.

    Science.gov (United States)

    Pont, Laura; Benavente, Fernando; Barbosa, José; Sanz-Nebot, Victoria

    2017-08-01

    This paper describes an on-line immunoaffinity solid-phase extraction capillary electrophoresis mass spectrometry (IA-SPE-CE-MS) method using an immunoaffinity sorbent with Fab' antibody fragments (Fab'-IA) for the analysis of serum transthyretin (TTR), a homotetrameric protein (M r ~56,000) involved in different types of amyloidosis. The IA sorbent was prepared by covalent attachment of Fab' fragments obtained from a polyclonal IgG antibody against TTR to succinimidyl silica particles. The Fab'-IA-SPE-CE-MS methodology was first established analyzing TTR standard solutions. Under optimized conditions, repeatability and reproducibility were acceptable, the method was linear between 1 and 25µgmL -1 , limits of detection (LODs) were around 0.5µgmL -1 (50-fold lower than by CE-MS, ~25µgmL -1 ) and different TTR conformations were observed (folded and unfolded). The applicability of the developed method to screen for familial amyloidotic polyneuropathy type I (FAP-I), which is the most common hereditary systemic amyloidosis, was evaluated analyzing serum samples from healthy controls and FAP-I patients. For the analysis of sera, the most abundant proteins were precipitated with 5% (v/v) of phenol before Fab'-IA-SPE-CE-MS. The current method enhanced our previous results for the analysis of TTR using intact antibodies immobilized on magnetic beads. It allowed a slight improvement on LODs (2-fold), the detection of proteoforms found at lower concentrations and the preparation of microcartridges with extended durability. Copyright © 2017. Published by Elsevier B.V.

  11. Concentração de bixina e lipídios em sementes de urucum da coleção do instituto agronômico (IAC Bixin and lipids content in annato seeds from collection of the instituto agronômico (IAC

    Directory of Open Access Journals (Sweden)

    Paulo Roberto Nogueira Carvalho

    2010-01-01

    Full Text Available Existe uma extensa variedade genética no urucum que são conhecidas por denominações como "focinho de rato", "cabeça de moleque", "peruana", "bico de pato", "amarela", "piave" entre outras. Todas são caracterizadas por propriedades como porte da planta, período de produção, forma e cores das cachopas, deiscência, etc. A última década tem sido marcada por um melhoramento genético, buscando maior produtividade e, principalmente, maior teor de pigmentos. O Instituto Agronômico (IAC comporta no Polo Regional Centro Norte, (Pindorama, SP, uma coleção de plantas de urucum, com mais de 25 acessos, que em trabalhos anteriores foram avaliadas quanto às suas características agronômicas. Contudo, os teores de bixina e lipídeos, que também são características importantes das sementes de urucum, pois afetam diretamente o rendimento industrial, não foram estudados. Este estudo teve como objetivo a validação de uma metodologia analítica de determinação de bixina e a caracterização da coleção do IAC quanto aos teores de bixina e lipídios. Os resultados indicaram que no método proposto houve linearidade na faixa de trabalho utilizada para a análise de sementes de urucum. Os limites de detecção e quantificação foram de 0,31 e 0,63 g de carotenóides totais expressos como bixina por 100 g de semente, respectivamente. O método foi preciso mas sensível a alterações na massa de amostra, tempo de extração e no coeficiente de absorção (. As árvores existentes na coleção possuem altos teores de bixina na semente, variando (em base seca de 3,12 ± 0,06% a 6,26 ± 0,06%. Os teores de lipídios variaram de 1,97 ± 0% a 3,98 ± 0,09%. Não foram observadas correlações entre as concentrações de bixina e de lipídios.Annato has wide genetic varieties that are known by different names including "focinho de rato", "cabeça de moleque", peruana, "bico de pato", yellow and piave. Different properties are used to characterize

  12. Métodos de analise dos danos da lagarta da espiga¹, em médias de gerações envolvendo IAC Maya e Zapalote Chico Method for analysis of damage of the corn earworm heliothis zea in generation means from IAC Maya and Zapalote Chico

    Directory of Open Access Journals (Sweden)

    Jorge Alberto Marques Rezende

    1982-01-01

    Full Text Available O milho Zapalote Chico 2451 (ZC 2451, referido na literatura como a melhor fonte de resistência à lagarta da espiga, Heliothis zea (Boddie, 1850, e o IAC Maya XII foram observados em condições de campo, juntamente com as gerações F1, e F2 resultantes do cruzamento de ambos, bem como os respectivos retrocruzamentos da população F1, para cada um dos pais, a fim de estudar métodos de análises de dados obtidos através da escala de dano revista por WIDSTROM e, conseqüentemente, fornecer subsídios para trabalhos de estudo da herança da resistência envolvendo esse cruzamento. Para analisar os dados, dividiram-se as notas de dano em quatro classes distintas agrupadas duas a duas, zero mais 1 e > 2, e zero e > 1, e aplicou-se o método do quiquadrado (c2 para verificar qual divisão melhor se ajustava. Os resultados revelaram que o grupo das classes zero mais 1 e > 2 apresentou melhor uniformidade dos dados entre as repetições dentro de cada tratamento. A análise da variância para cada classe de dano, separadamente, apresentou valores de F altamente significativos para as classes zero e zero mais 1, enquanto para as classes > 1 e > 2, os mesmos não permitiram diferenciar os tratamentos. Entre as classes zero e zero mais 1, esta última revelou maior significância e melhor precisão dos dados. O milho ZC 2451, quando comparado com a variedade IAC Maya XII, exibiu boa resistência à lagarta da espiga nas condições de Campinas (SP, resistência essa relacionada com fatores de não preferência e/ou antibiose, devido ã maior porcentagem de espigas não danificadas do ZC 2451.The line Zapalote Chico 2451 (ZC 2451 resistant to the corn earworm, Heliothis zea, the commercial synthetic Brazilian variety IAC Maya XII, the F1 and F2 obtained with their cross, and the two back crosses between the F1 and both parents, were planted in the field in a randomized block with 10 replications. The earworm damage done to the ears was graded

  13. Goiaba (psidium guajava L.) cultivar IAC-4 : carotenoides e outras propriedades, mudanças durante processamento e estocagem

    OpenAIRE

    Marisa Padula

    1983-01-01

    Resumo: Através da cromatografia em coluna e em camada delgada, espectrometria de absorção visível e reações químicas, os carotenóides na goiaba Cultivar IAC-4 foram identificados como: 8-caroteno, ζ-caroteno, γ-caroteno, zeinoxantina, licopeno, 5,6,5',6'- diepóxi-B-caroteno e 5,8-epóxi-3,31,4-trihidroxi-3-caroteno. O principal pigmento foi o licopeno, correspondendo a 86% de 62 γg/g de carotenóides totais. O teor de B-caroteno foi 3,7 γg/g, conse- qüentemente o valor de v...

  14. Extrasynaptic location of laminin beta 2 chain in developing and adult human skeletal muscle

    DEFF Research Database (Denmark)

    Wewer, U M; Thornell, L E; Loechel, F

    1997-01-01

    and Becker muscular dystrophy. Immunoaffinity chromatography of muscle extracts with a monoclonal antibody to the laminin alpha 2 chain followed by immunoblotting with various antibodies to the beta 2 chain demonstrated the presence of the laminin-4 (alpha 2-beta 2-gamma 1) isoform. Together the present...

  15. Determination of aflatoxins in medicinal plants by high-performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Siddique, Nadeem A; Mujeeb, Mohd; Ahmad, Sayeed; Panda, Bibhu P; Makhmoor, Mohd

    2013-01-01

    The intention of the proposed work is to study the presence of the aflatoxins B1, B2, G1 and G2 in medicinal plants, namely Mucuna pruriens, Delphinium denudatum and Portulaca oleraceae. The aflatoxins were extracted, purified by immunoaffinity column chromatography and analysed by high-performance liquid chromatography-tandem quadrupole mass spectrometry with electrospray ionisation (HPLC-MS/MS). Fungal count was carried out in PDA media. A good linear relationship was found for AFB1, AFB2, AFG1 and AFG2 at 1-10 ppb (r>0.9995). The analyte accuracy under three different spiking levels was 86.7-108.1 %, with low per cent relative standard deviations in each case. The aflatoxins can be separated within 5 to7 min using an Agilent XDB C18-column. We found that AFB1 and AFB2 were in trace amounts below the detection limit in M. pruriens whilst they were not detected in D. denudatum. P. oleraceae was found to be contaminated with AFB1 and AFB2. AFG1 and AFG2 were not detected in M. pruriens, P. oleraceae and were below the detection limit in D. denudatum. This was consistent with very low numbers of fungal colonies observed after 6 hr of incubation. The analytical method developed is simple, precise, accurate, economical and can be effectively used to determine the aflatoxins in medicinal plants and therefore to control the quality of products. The aflatoxin levels in the plant extracts examined were related to the minimal fungal load in the medicinal plants examined.

  16. Quantitative analysis of factor P (Properdin) in monkey serum using immunoaffinity capturing in combination with LC-MS/MS.

    Science.gov (United States)

    Gao, Xinliu; Lin, Hui; Krantz, Carsten; Garnier, Arlette; Flarakos, Jimmy; Tse, Francis L S; Li, Wenkui

    2016-01-01

    Factor P (Properdin), an endogenous glycoprotein, plays a key role in innate immune defense. Its quantification is important for understanding the pharmacodynamics (PD) of drug candidate(s). In the present work, an immunoaffinity capturing LC-MS/MS method has been developed and validated for the first time for the quantification of factor P in monkey serum with a dynamic range of 125 to 25,000 ng/ml using the calibration standards and QCs prepared in factor P depleted monkey serum. The intra- and inter-run precision was ≤7.2% (CV) and accuracy within ±16.8% (%Bias) across all QC levels evaluated. Results of other evaluations (e.g., stability) all met the acceptance criteria. The validated method was robust and implemented in support of a preclinical PK/PD study.

  17. Development of an Ultrasonication-Assisted Extraction Based HPLC With a Fluorescence Method for Sensitive Determination of Aflatoxins in Highly Acidic Hibiscus sabdariffa

    Directory of Open Access Journals (Sweden)

    Xiaofei Liu

    2018-04-01

    Full Text Available The high acidity and complex components of Hibiscus sabdariffa have provided major challenges for sensitive determination of trace aflatoxins. In this study, sample pretreatment of H. sabdariffa was systematically developed for sensitive high performance liquid chromatography-fluorescence detection (HPLC-FLD after ultrasonication-assisted extraction, immunoaffinity column (IAC clean-up and on-line post-column photochemical derivatization (PCD. Aflatoxins B1, B2, G1, G2 were extracted from samples by using methanol/water (70:30, v/v with the addition of NaCl. The solutions were diluted 1:8 with 0.1 M phosphate buffer (pH 8.0 to negate the issues of high acidity and matrix interferences. The established method was validated with satisfactory linearity (R > 0.999, sensitivity (limits of detection (LODs and limits of quantitation (LOQs of 0.15–0.65 and 0.53–2.18 μg/kg, respectively, precision (RSD <11%, stability (RSD of 0.2–3.6%, and accuracy (recovery rates of 86.0–102.3%, which all met the stipulated analytical requirements. Analysis of 28 H. sabdariffa samples indicated that one sample incubated with Aspergillus flavus was positive with aflatoxin B1 (AFB1 at 3.11 μg/kg. The strategy developed in this study also has the potential to reliably extract and sensitively detect more mycotoxins in other complex acidic matrices, such as traditional Chinese medicines, foodstuffs, etc.

  18. Multiplexed Quantification of Proglucagon-Derived Peptides by Immunoaffinity Enrichment and Tandem Mass Spectrometry after a Meal Tolerance Test

    DEFF Research Database (Denmark)

    Lee, Anita Y H; Chappell, Derek L; Bak, Monika J

    2016-01-01

    . Participants fasted overnight and were either given a meal (n = 8) or continued to fast (n = 4), with multiple blood collections over the course of 3 h. Plasma samples were analyzed by microflow immunoaffinity (IA)-LC-MS/MS with an isotope dilution strategy. RESULTS: Assay performance characteristics were...... examined and established during analytical validation for all peptides. Intra- and interassay imprecision were found to be 2.2%-10.7% and 6.8%-22.5%, respectively. Spike recovery was >76%, and dilution linearity was established up to a 16-fold dilution. Immediately after the meal tolerance test, GLP-1...... and oxyntomodulin concentrations increased and had an almost identical temporal relationship, and glucagon concentrations increased with a slight delay. CONCLUSIONS: IA-LC-MS/MS was used for the simultaneous and selective measurement of PGDPs. This work includes the first indication of the physiological...

  19. Growth curves of coffee fruits Obatã IAC 1669-20 in different alignments planting /Curvas de crescimento do fruto de cafeeiro cv. Obatã IAC 1669-20 em diferentes alinhamentos de plantio

    Directory of Open Access Journals (Sweden)

    Clovis Alberto Volpe

    2011-03-01

    Full Text Available The growth of the coffee fruit is highly dependent on physiological and environmental factors. Environmental factors that most influence the yield of coffee during the critical growth stages are the minimum and maximum temperatures of air, which are affected by solar radiation and depend on the apparent path of the sun. This research work correlated dry mass versus fresh mass, and, fresh and dry mass as function of days after flowering of fruit coffee cv. Obatã IAC 1669-20 planted in three different alignments based on the apparent trajectory of the sun, in Jaboticabal, SP. The planting was aligned according to the apparent path of the sun. There were three treatments with four replications, a total of twelve plots, each plot with one hundred plants of coffee, each treatment corresponded to an alignment of planting. The three alignments used showed no differences with respect the average fresh and dry mass. The growth rate of fruit, in fresh weight, was higher in the exponential phase, and in dry mass was higher in the linear stage. The dry weight (DW can be estimated from the fresh weight (FW using the model: . The sigmoidal model that represents the fruit growth in of coffee plants in fresh and/or dry mass in terms of days after flowering (DAF was: .O crescimento do fruto do cafeeiro é altamente dependente de fatores fisiológicos e ambientais. Os fatores ambientais que mais interferem na produtividade do cafeeiro durante os estádios fenológicos críticos são as temperaturas mínimas e máximas do ar, as quais são efeitos da radiação solar e dependente da trajetória aparente do sol. Este trabalho correlacionou massa seca versus massa fresca, e massas fresca e seca em função de dias após o florescimento, de fruto de cafeeiro cv. Obatã IAC 1669-20 plantados em três diferentes alinhamentos baseados na trajetória aparente do Sol, em Jaboticabal, SP. Foram três tratamentos, com quatro repetições, num total de doze parcelas, e cada

  20. Analysis of human serum by liquid chromatography-mass spectrometry: improved sample preparation and data analysis.

    Science.gov (United States)

    Govorukhina, N I; Reijmers, T H; Nyangoma, S O; van der Zee, A G J; Jansen, R C; Bischoff, R

    2006-07-07

    Discovery of biomarkers is a fast developing field in proteomics research. Liquid chromatography coupled on line to mass spectrometry (LC-MS) has become a powerful method for the sensitive detection, quantification and identification of proteins and peptides in biological fluids like serum. However, the presence of highly abundant proteins often masks those of lower abundance and thus generally prevents their detection and identification in proteomics studies. To perform future comparative analyses of samples from a serum bank of cervical cancer patients in a longitudinal and cross-sectional manner, methodology based on the depletion of high-abundance proteins followed by tryptic digestion and LC-MS has been developed. Two sample preparation methods were tested in terms of their efficiency to deplete high-abundance serum proteins and how they affect the repeatability of the LC-MS data sets. The first method comprised depletion of human serum albumin (HSA) on a dye ligand chromatographic and immunoglobulin G (IgG) on an immobilized Protein A support followed by tryptic digestion, fractionation by cation-exchange chromatography, trapping on a C18 column and reversed-phase LC-MS. The second method included depletion of the six most abundant serum proteins based on multiple immunoaffinity chromatography followed by tryptic digestion, trapping on a C18 column and reversed-phase LC-MS. Repeatability of the overall procedures was evaluated in terms of retention time and peak area for a selected number of endogenous peptides showing that the second method, besides being less time consuming, gave more repeatable results (retention time: <0.1% RSD; peak area: <30% RSD). Application of an LC-MS component detection algorithm followed by principal component analysis (PCA) enabled discrimination of serum samples that were spiked with horse heart cytochrome C from non-spiked serum and the detection of a concentration trend, which correlated to the amount of spiked horse heart

  1. Phenylboronic acid immunoaffinity reactor coupled with flow injection chemiluminescence for determination of {alpha}-fetoprotein

    Energy Technology Data Exchange (ETDEWEB)

    Wu Yafeng [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China); Zhuang Yafeng [Department of Chemistry, Changzhou Institute of Technology, Changzhou 213022 (China); Liu Songqin [Jiangsu Provincial Key Lab of Biomaterials and Biodevices, School of Chemistry and Chemical Engineering, Southeast University, Nanjing 210096 (China)], E-mail: liusq@seu.edu.cn; He Lin [Department of Chemistry, North Carolina State University, Raleigh, NC 27695-8204 (United States)

    2008-12-23

    A reusable and sensitive immunoassay based on phenylboronic acid immunoaffinity reactor in combination with flow injection chemiluminescence (CL) for determination of glycoprotein was described. The reactor was fabricated by immobilizing 3-aminophenylboronic acid (APBA) on glass microbeads with {gamma}-glycidoxypropyltrimethoxysilane (GPMS) as linkage. The {alpha}-fetoprotein (AFP) could be easily immobilized on the APBA coated beads through sugar-boronic interaction. After an off-line incubation, the mixture of the analyte AFP with horseradish peroxidase-labeled AFP antibody (HRP-anti-AFP) was injected into the reactor. This led the trapping of free HRP-anti-AFP by the surface coated AFP on glass beads. The trapped HRP-anti-AFP was detected by chemiluminescence due to its sensitizing effect on the reaction of luminol and hydrogen peroxide. Under optimal conditions, the chemiluminescent signal was proportional to AFP concentration in the range of 10-100 ng mL{sup -1}. The whole assay process including regeneration of the reactor could be completed within 31 min. The proposed system showed acceptable detection and fabrication reproducibility, and the results obtained with the present method were in acceptable agreement with those from parallel single-analyte test of practical clinical sera. The described method enabled a low-cost, time saving and was potential to detect the serum AFP level in clinical diagnosis.

  2. Análise do regime hídrico de Patos-PB por meio do Índice de Anomalia de Chuvas (IAC

    Directory of Open Access Journals (Sweden)

    M. F. A. Alves

    2015-12-01

    Full Text Available A seca é um fenômeno natural que o ser humano não consegue impedir que ocorra. Nesse sentido, a presente pesquisa tem por objetivo, analisar o comportamento do regime hídrico do município de Patos interior da Paraíba, no período de 1994 a 2009 utilizando o IAC. Para o desenvolvimento da pesquisa, realizou-se um levantamento pluviométrico de 15 anos obtidos no site da Agência Executiva de Gestão das Águas da Paraíba (AESA de 1994 a 2009. Os dados foram disponibilizados em planilha eletrônica do Microsoft Excel com informações diárias, mensais e anuais e por último foi analisado o comportamento das precipitações através do Índice de Anomalia de Chuva (IAC, que é bastante simples e empregado para avaliação dos períodos secos ou úmidos. Pelo o estudo observou-se que apenas 2009 apresentou um mês (abril, como extremamente úmido e os demais anos foram classificados como muito úmidos, úmidos e secos. O ano mais seco foi 1998 que apresentou anomalias negativas de fevereiro a maio, seguido de 1999 com anomalias negativas em fevereiro e abril do período chuvoso. Dos resultados se percebe que as principais chuvas que ocorrem sob a região estudada caem sobre a terra de forma mal distribuída e irregular, e que o índice pluviométrico da região, se comparado com outras regiões áridas do planeta, o semiárido paraibano é um dos que mais chove em todo mundo, deixando claro que a falta de água que assola os nordestinos são decorrentes das características das chuvas. Percebe-se que apenas 2009 apresentou mês tido como extremamente úmido e isso não é caraterístico da região, devendo-se, sobretudo a modelos de estabilização da atmosfera por eventos meteorológicos que provocaram as chuvas fora do período chuvoso de Patos. Analysis of water regime of Patos-PB through Rainfall Anomaly Index (RAIAbstract: Drought is a natural phenomenon that humans can't prevent that from occurring. In this sense, this research aims

  3. Chromatography.

    Science.gov (United States)

    Brantley, L. Reed, Sr.; Demanche, Edna L.; Klemm, E. Barbara; Kyselka, Will; Phillips, Edwin A.; Pottenger, Francis M.; Yamamoto, Karen N.; Young, Donald B.

    This booklet presents some activities on chromatography. Directions for preparing leaf pigment extracts using alcohol are given, and paper chromatography and thin-layer chromatography are described as modifications of the basic principles of chromatography. (KHR)

  4. Identification and Quantification of Several Mammalian Steroid Hormones in Plants by UPLC-MS/MS

    Czech Academy of Sciences Publication Activity Database

    Simerský, Radim; Novák, Ondřej; Morris, David; Pouzar, Vladimír; Strnad, Miroslav

    2009-01-01

    Roč. 28, č. 2 (2009), s. 125-136 ISSN 0721-7595 R&D Projects: GA AV ČR KAN200380801 Institutional research plan: CEZ:AV0Z50380511; CEZ:AV0Z40550506 Keywords : Ultra-performance liquid chromatography (UPLC) * Tandem mass spectrometry (MS/MS) * Immunoaffinity purification * Steroids * Plant extracts * Digitalis purpurea * Nicotiana tabacum * Inula helenium Subject RIV: EC - Immunology Impact factor: 2.438, year: 2009

  5. Avaliação de compostos fenólicos em geléia de uva produzida com a variedade IAC-138-22 (máximo)

    OpenAIRE

    Luciula Lemos Lima Morelli

    2011-01-01

    Resumo: O presente trabalho buscou avaliar a presença de compostos fenólicos antioxidantes em geleia de uva produzida com a variedade Máximo (IAC-138-22), por meio de (1) métodos colorimétricos e (2) cromatografia liquida de alta eficiência. Foram produzidas 3 formulações de geleia com a nova variedade e 3 outras com a mistura entre as variedades Niágara Rosada e Isabel, para efeito comparativo. As formulações diferiam em relação à quantidade de casca de uva incorporada à formulação, sendo a ...

  6. Evaluation of extraction methods for ochratoxin A detection in cocoa beans employing HPLC.

    Science.gov (United States)

    Mishra, Rupesh K; Catanante, Gaëlle; Hayat, Akhtar; Marty, Jean-Louis

    2016-01-01

    Cocoa is an important ingredient for the chocolate industry and for many food products. However, it is prone to contamination by ochratoxin A (OTA), which is highly toxic and potentially carcinogenic to humans. In this work, four different extraction methods were tested and compared based on their recoveries. The best protocol was established which involves an organic solvent-free extraction method for the detection of OTA in cocoa beans using 1% sodium hydrogen carbonate (NaHCO3) in water within 30 min. The extraction method is rapid (as compared with existing methods), simple, reliable and practical to perform without complex experimental set-ups. The cocoa samples were freshly extracted and cleaned-up using immunoaffinity column (IAC) for HPLC analysis using a fluorescence detector. Under the optimised condition, the limit of detection (LOD) and limit of quantification (LOQ) for OTA were 0.62 and 1.25 ng ml(-1) respectively in standard solutions. The method could successfully quantify OTA in naturally contaminated samples. Moreover, good recoveries of OTA were obtained up to 86.5% in artificially spiked cocoa samples, with a maximum relative standard deviation (RSD) of 2.7%. The proposed extraction method could determine OTA at the level 1.5 µg kg(-)(1), which surpassed the standards set by the European Union for cocoa (2 µg kg(-1)). In addition, an efficiency comparison of IAC and molecular imprinted polymer (MIP) column was also performed and evaluated.

  7. High levels of inactive thymidine kinase 1 polypeptide detected in sera from dogs with solid tumours by immunoaffinity methods: implications for in vitro diagnostics.

    Science.gov (United States)

    Kiran Kumar, J; Sharif, H; Westberg, S; von Euler, H; Eriksson, S

    2013-09-01

    Determination of serum thymidine kinase 1 (STK1) activity has been used as a proliferation marker for neoplastic diseases in both human and veterinary medicine. The purpose of this study was to determine STK1 activity and enzyme levels in different dog tumours. Serum samples from three dogs with leukaemia, five with lymphoma, 21 with solid tumours and 18 healthy dogs were analyzed for STK1 activity, using an optimized [(3)H]-deoxythymidine (dThd) phosphorylation assay, and for STK1 protein levels using an immunoaffinity/western blot assay. STK1 activity in dogs with haematological tumours was significantly higher than in the solid tumour and healthy dog groups (mean ± standard deviation [SD] = 65 ± 79, 1.1 ± 0.5, and 1.0 ± 0.4 pmol/min/mL, respectively). Serum samples were analyzed after immunoaffinity isolation by western blot and the TK1 26 kDa band intensities quantified revealing that concentrations were significantly higher in dogs with haematological tumours and solid tumours compared to healthy dogs (mean ± SD=33 ± 12, 30 ± 13, and 10 ± 5 ng/mL, respectively). Pre-incubation with the reducing agent dithioerythritol (DTE) showed a decrease in STK1 activity and protein levels in most samples, but an increase of about 20% in sera from healthy dogs and from those with haematological malignancies. Compared to animals with solid tumours, the specific STK1 activity (nmol [(3)H]-deoxythymidine monophosphate (dTMP)/min/mg of TK1 protein of 26 kDa) was 30-fold higher in haematological malignancies and 2.5-fold higher in healthy dogs, respectively. The results demonstrate that there is a large fraction of inactive TK1 protein, particularly in sera from dogs with solid tumours. The findings are important in the use of STK1 as a biomarker. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Uso de misturas de adubos contendo ou não enxofre na adubação do cultivar IAC 16 de algodoeiro The effect of sulfur on 'IAC 16' cotton

    Directory of Open Access Journals (Sweden)

    Nelson M. Silva

    1981-01-01

    Full Text Available Durante quatro anos agrícolas, foi conduzido com o algodoeiro - cultivar IAC 16, ensaio de caráter permanente, de competição de misturas de adubos contendo ou não enxofre, em Latossolo Roxo, ácido, de baixa fertilidade, anteriormente ocupado com pastagem não adubada, no municipio de Guaíra (SP. A combinação de produtos comerciais, como sulfato de amônio, salitre-do-chile, nitrato de amônio, superfosfatos simples e triplo, e cloreto de potássio, permitiu ceder às plantas N e K em doses constantes e P e S em doses variáveis. No primeiro e no último ano agrícola, foram aplicadas pequenas quantidades de calcário dolomítico. A produtividade das plantas no primeiro ano agrícola foi muito baixa, mesmo nos níveis altos de adubação, o que confirma o risco de insucesso que se corre cultivando o algodoeiro em início de correção de solo ácido. O efeito do fósforo sobre a produção das plantas praticamente inexistiu nesse ano e foi de natureza quadrática após sucessivos acúmulos de adubos. A ação do enxofre se fez sentir desde o primeiro ano, aumentando com o tempo e com a efetivação do efeito das calagens. O superfosfato simples comportou-se como adubo misto, tendo proporcionado aumentos no teor de Ca trocável do solo e na concentração de Ca e S na folha do algodoeiro, após aplicações sucessivas. Através dos anos, proporcionou produtividades sistematicamente superiores às devidas ao superfosfato triplo. As maiores produções, entretanto, foram obtidas com a inclusão do sulfato de amônio em cobertura. Não se observou correlação satisfatória entre concentração de nutrientes na planta e níveis de produtividade, uma vez que K, S, N e P se acumularam nas folhas das plantas que não receberam PeSna adubação, devido provavelmente à pouca carga de capulhos formada nesse caso.The influence of the repeated applications of fertilizer mixtures containing P and S and of mixtures without S, was studied by a

  9. Caracterização e hidrólise in vitro da globulina principal de grão-de-bico (Cicer arietinum L., var. IAC-Marrocos Characterization and in vitro tryptic hydrolysis of the major globulin from chickpea (Cicer arietinum L.

    Directory of Open Access Journals (Sweden)

    Valdir A. Neves

    2004-03-01

    Full Text Available No presente estudo procedeu-se ao isolamento e caracterização da fração globulina majoritária (11 S de grão-de-bico, var. IAC-Marrocos. A globulina majoritária extraída foi isolada por cromatografia de filtração em gel e de troca-iônica mostrando apenas uma banda de proteína na eletroforese em gel de poliacrilamida. A globulina majoritária, após passagem em coluna de Sephadex, revelou duas bandas protéicas de 55 e 52,5kDa e três bandas menores em gel de poliacrilamida dodecilsulfato de sódio. Na presença de 2-mercaptoetanol 6 polipeptídios na faixa de 18 a 42kDa foram revelados na eletroforese. A globulina isolada foi submetida à ação da tripsina e quimotripsina onde a forma nativa mostrou-se resistente à ação enzimática enquanto o aquecimento (96 e 121°C/15min não foi suficiente para aumentar a susceptibilidade à hidrólise, significativamente. Adição de NaCl 0,3M levou a um aumento da estabilidade estrutural com menor susceptibilidade à digestão proteolítica, fato em parte perdido com o aquecimento. As hidrólises foram acompanhadas por eletroforese em gel de poliacrilamida dodecilsulfato de sódio.The isolation and characterization of the major globulin fraction (11 S from Chickpea, vc IAC-Marrocos, were evaluated. The major globulin was extracted, isolated by gel filtration and ion-exchange chromatography showing only one protein band on PAGE. The globulin, after Sephadex elution, revealed two protein bands of 55 and 52.5kDa and three minor bands on SDS-PAGE. In the presence of 2-mercaptoethanol six polypeptides were revealed on SDS-PAGE in the range of 18 to 42kDa. The isolated native globulin shown to be resistant to trypsin and chymotrypsin however heating at 96 and 121ºC/15min was not sufficient to increase the hydrolysis significantly. The proteolytic susceptibility of the enzymes was reduced by 0.3M NaCl addition at the assay. The salt concentration was sufficient to stabilize the native protein

  10. High-sensitivity direct analysis of aflatoxins in peanuts and cereal matrices by ultra-performance liquid chromatography with fluorescence detection involving a large volume flow cell.

    Science.gov (United States)

    Oulkar, Dasharath; Goon, Arnab; Dhanshetty, Manisha; Khan, Zareen; Satav, Sagar; Banerjee, Kaushik

    2018-04-03

    This paper reports a sensitive and cost effective method of analysis for aflatoxins B1, B2, G1 and G2. The sample preparation method was primarily optimised in peanuts, followed by its validation in a range of peanut-processed products and cereal (rice, corn, millets) matrices. Peanut slurry [12.5 g peanut + 12.5 mL water] was extracted with methanol: water (8:2, 100 mL), cleaned through an immunoaffinity column and thereafter measured directly by ultra-performance liquid chromatography-fluorescence (UPLC-FLD) detection, within a chromatographic runtime of 5 minutes. The use of a large volume flow cell in the FLD nullified the requirement of any post-column derivatisation and provided the lowest ever reported limits of quantification of 0.025 for B1 and G1 and 0.01 μg/kg for B2 and G2. The single laboratory validation of the method provided acceptable selectivity, linearity, recovery and precision for reliable quantifications in all the test matrices as well as demonstrated compliance with the EC 401/2006 guidelines for analytical quality control of aflatoxins in foodstuffs.

  11. Plasma chromatography

    International Nuclear Information System (INIS)

    Anon.

    1984-01-01

    This book examines the fundamental theory and various applications of ion mobility spectroscopy. Plasma chromatography developed from research on the diffusion and mobility of ions. Topics considered include instrument design and description (e.g., performance, spectral interpretation, sample handling, mass spectrometry), the role of ion mobility in plasma chromatography (e.g., kinetic theory of ion transport), atmospheric pressure ionization (e.g., rate equations), the characterization of isomers by plasma chromatography (e.g., molecular ion characteristics, polynuclear aromatics), plasma chromatography as a gas chromatographic detection method (e.g., qualitative analysis, continuous mobility monitoring, quantitative analysis), the analysis of toxic vapors by plasma chromatography (e.g., plasma chromatograph calibration, instrument control and data processing), the analysis of semiconductor devices and microelectronic packages by plasma chromatography/mass spectroscopy (e.g., analysis of organic surface contaminants, analysis of water in sealed electronic packages), and instrument design and automation (hardware, software)

  12. Immunoaffinity Knockout of Saponin Glycosides from Asparagus racemosus to Assess Anti-lipid Peroxidation.

    Science.gov (United States)

    Onlom, Churanya; Phrompittayarat, Watoo; Putalun, Waraporn; Waranuch, Neti; Ingkaninan, Kornkanok

    2017-07-01

    Asparagus racemosus Willd (Asparagaceae family), known as Shatavari, is important in Ayurveda and traditional Thai medicines. The saponin glycosides, shatavarin I and IV are major constituents in its roots and may be responsible for their actions including protection against lipid peroxidation and carcinogenesis. To develop an immunoaffinity column for isolating compounds with structures related to shatavarin IV from crude extracts of A. racemosus root. The monoclonal antibody recognising shatavarin IV (mAbShavIV) was coupled to an Affi-Gel Hz gel to isolate compounds with structures related to shatavarin IV from the other components of crude extracts of A. racemosus root. The saponin glycosides in each fraction were analysed by mAbShavIV ELISA and LC-MS/MS. The pooled wash-through fractions contained 3% of loaded mAbShavIV reactive saponin glycosides, while eluted fractions released ~ 90% of shatavarin saponin glycosides in a single step. Using thiobarbiturate (TBARs) to measure lipid-peroxidation, the extract, and the pooled wash-through fractions showed moderate protection against Cu + -induced oxidation of human low density lipoprotein (LDL) (IC 50 11.3 ± 1.4 and 12.6 ± 0.9 μg/mL, respectively). In contrast, the saponin glycosides eluted from the mAbShavIV-column had weaker protectant (IC 50 29.7 ± 1.8 μg/mL) suggesting that A. racemosus shatavarins do not inhibit carcinogenesis through preventing lipid peroxidation. The strategy described here demonstrates its utility for isolating a group of related compounds from the rest of the extract with selectivity and recovery rate. Pharmacological efficacy and synergistic effects of the components obtained can be further investigated. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  13. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

  14. Analysis of Serum Total and Free PSA Using Immunoaffinity Depletion Coupled to SRM: Correlation with Clinical Immunoassay Tests

    Science.gov (United States)

    Liu, Tao; Hossain, Mahmud; Schepmoes, Athena A.; Fillmore, Thomas L.; Sokoll, Lori J.; Kronewitter, Scott R.; Izmirlian, Grant; Shi, Tujin; Qian, Wei-Jun; Leach, Robin J.; Thompson, Ian M.; Chan, Daniel W.; Smith, Richard D.; Kagan, Jacob; Srivastava, Sudhir; Rodland, Karin D.; Camp, David G.

    2012-01-01

    Recently, selected reaction monitoring mass spectrometry (SRM-MS) has been more frequently applied to measure low abundance biomarker candidates in tissues and biofluids, owing to its high sensitivity and specificity, simplicity of assay configuration, and exceptional multiplexing capability. In this study, we report for the first time the development of immunoaffinity depletion-based workflows and SRM-MS assays that enable sensitive and accurate quantification of total and free prostate-specific antigen (PSA) in serum without the requirement for specific PSA antibodies. Low ng/mL level detection of both total and free PSA was consistently achieved in both PSA-spiked female serum samples and actual patient serum samples. Moreover, comparison of the results obtained when SRM PSA assays and conventional immunoassays were applied to the same samples showed good correlation in several independent clinical serum sample sets. These results demonstrate that the workflows and SRM assays developed here provide an attractive alternative for reliably measuring candidate biomarkers in human blood, without the need to develop affinity reagents. Furthermore, the simultaneous measurement of multiple biomarkers, including the free and bound forms of PSA, can be performed in a single multiplexed analysis using high-resolution liquid chromatographic separation coupled with SRM-MS. PMID:22846433

  15. Improved sensitivity of ochratoxin A analysis in coffee using high-performance liquid chromatography with hybrid triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS).

    Science.gov (United States)

    Kokina, Aija; Pugajeva, Iveta; Bartkevics, Vadims

    2016-01-01

    A novel and sensitive method utilising high-performance liquid chromatography coupled to triple quadrupole-linear ion trap mass spectrometry (LC-QqQLIT-MS/MS) was developed in order to analyse the content of ochratoxin A (OTA) in coffee samples. The introduction of the triple-stage MS scanning mode (MS(3)) has been shown to increase greatly sensitivity and selectivity by eliminating the high chromatographic baseline caused by interference of complex coffee matrices. The analysis included the sample preparation procedure involving extraction of OTA using a methanol-water mixture and clean-up by immunoaffinity columns and detection using the MS(3) scanning mode of LC-QqQLIT-MS/MS. The proposed method offered a good linear correlation (r(2) > 0.998), excellent precision (RSD coffee beans and espresso beverages was 0.010 and 0.003 µg kg(-1), respectively. The developed procedure was compared with traditional methods employing liquid chromatography coupled to fluorescent and tandem quadrupole detectors in conjunction with QuEChERS and solid-phase extraction. The proposed method was successfully applied to the determination of OTA in 15 samples of coffee beans and in 15 samples of espresso coffee beverages obtained from the Latvian market. OTA was found in 10 samples of coffee beans and in two samples of espresso in the ranges of 0.018-1.80 µg kg(-1) and 0.020-0.440 µg l(-1), respectively. No samples exceeded the maximum permitted level of OTA in the European Union (5.0 µg kg(-1)).

  16. Caracterização agronômica e pungência em pimenta de cheiro Agronomic traits and pungency of chilli pepper

    Directory of Open Access Journals (Sweden)

    Carolina I Domenico

    2012-09-01

    údo de capsaicina, resultado inédito para uma pimenta de cheiro brasileira.Nine accessions of the Active Capsicum chinense Germplasm Bank of Instituto Agronômico were characterized and evaluated in climate and soil conditions of Campinas, São Paulo state, Brazil. The experiment was carried out from January to October 2010. The experimental design was randomized blocks, with nine treatments, five replications and eight plants per plot. Evaluated traits were plant height, plant growth habit, first flower anthesis, fruit yield, fresh fruit weight, fruit height and width, capsaicin content, ripe fruit color, fruit shape and fruit surface. For fruit and plant characterization were considered the four central plants of each plot; for capsaicin content evaluation were used three samples of five fruits of each accession. Capsaicin content was measured by ultra-high pressure liquid chromatography. Plant height ranged from 1.13 to 0.85 m. The most accessions presented compact growth habit of plants. Accessions IAC 1644, IAC 1645 and IAC 1643 were the earliest for anthesis of first flower. IAC 1646 showed high fruit yield, fruit width and fresh weight, and IAC 1641 showed the longest fruits. IAC 1552 ('Murupi' stood out with highest capsaicin content, outperforming IAC 1646 ('Scotch Bonnet' and IAC 1644 ('Fidalga', habanero types. Fruits presented yellow, orange, salmon and red colors. The fruits presented the elongated, round, triangular, campanulated and blocked shape. The fruit surface was characterized as smooth, semi-rough and rough. In the climate and soil conditions where the research was developed and, regarding the accessions evaluated, there was high variability in chili peppers for agronomic traits and capsaicin content. IAC 1552 stood out with highest capsaicin content, first result for a Brazilian chilli pepper.

  17. Chromatography resin support

    Science.gov (United States)

    Dobos, James G.

    2002-01-01

    An apparatus and method of using an improved chromatography resin support is disclosed. The chromatography support platform is provided by a stainless steel hollow cylinder adapted for being inserted into a chromatography column. An exterior wall of the stainless steel cylinder defines a groove for carrying therein an "O"-ring. The upper surface of the stainless steel column is covered by a fine stainless steel mesh welded to the edges of the stainless steel cylinder. When placed upon a receiving ledge defined within a chromatography column, the "O"-ring provides a fluid tight seal with the inner edge wall of the chromatography cylinder. The stainless steel mesh supports the chromatography matrix and provides a back flushable support which is economical and simple to construct.

  18. Analysis of cocoa products for ochratoxin A and aflatoxins.

    Science.gov (United States)

    Turcotte, Anne-Marie; Scott, Peter M; Tague, Brett

    2013-08-01

    Eighty-five samples of cocoa products sampled in Canada were analysed for ochratoxin A (OTA) and aflatoxins in 2011-2012. Inclusion of the aflatoxins in this survey required additional method development. Chocolate was extracted with methanol-water plus NaCl, while for cocoa two successive extractions with methanol and methanol-water were made. Extracts were cleaned on an AflaOchra immunoaffinity column (IAC). Determination was by reversed phase high performance liquid chromatography (HPLC). Detection of the aflatoxins was with a post-column photochemical reactor and of OTA by fluorescence detection. Mean limits of quantification (LOQ) of chocolate and cocoa powders were 0.16 ng/g (OTA) and 0.07 ng/g (aflatoxin B1), respectively. Survey results showed that the incidences of OTA above the LOQ in natural cocoa were 15/15 (mean 1.17 ng/g), 20/21 for alkalized cocoa (mean 1.06 ng/g), 9/9 for baking chocolate (mean 0.49 ng/g), 20/20 for dark chocolate (mean 0.39 ng/g), 7/10 for milk chocolate (mean 0.19 ng/g), 5/5 for cocoa liquor (mean 0.43 ng/g), and 0/5 for cocoa butter. These results confirm our previous work with OTA. In the same samples, incidences of aflatoxin B1 above the LOQ were 14/15 for natural cocoa (mean 0.86 ng/g), 20/21 for alkalized cocoa (mean 0.37 ng/g), 7/9 for baking chocolate (mean 0.22 ng/g), 16/20 for dark chocolate (mean 0.19 ng/g), 7/10 for milk chocolate (mean 0.09 ng/g), 4/5 for cocoa liquor (mean 0.43 ng/g), and 0/5 for cocoa butter. Both aflatoxins and OTA were confirmed by HPLC-MS/MS when OTA or aflatoxin levels found were above 2 ng/g in cocoa.

  19. Alterações morfológicas foliares em abacaxizeiros cv. IAC "Gomo-de-mel" micropropagados e aclimatizados em diferentes condições de luminosidade Morphological alterations in leave of micropropagated pineapple plants cv. IAC "Gomo-de-mel" acclimatizated in different conditions of luminosity

    Directory of Open Access Journals (Sweden)

    Katherine Derlene Batagin

    2009-03-01

    Full Text Available Plantas micropropagadas geralmente apresentam dificuldades de adaptação ao meio ex vitro, sendo muitas vezes submetidas a processos de rustificação para minimizar os impactos decorrentes da mudança de ambiente. Uma vez que a folha e seus anexos destacam-se como importantes indicativos das estratégias adaptativas das plantas a ambientes adversos, este trabalho teve por objetivo comparar a anatomia foliar de plantas de abacaxi cv. IAC "Gomo-de-mel" cultivadas in vitro com microplantas aclimatizadas em diferentes condições de luminosidade, sob telado com 50% de sombreamento e em pleno sol para verificar a necessidade do processo de rustificação para este cultivar. Avaliações por meio de microscopia de luz e eletrônica de varredura da epiderme foliar, demonstraram aumento na densidade de escamas em ambas as superfícies das folhas, em microplantas dos ambientes ex vitro, principalmente em relação às que foram expostas diretamente ao sol. Observou-se ainda, aumento no espessamento da cutícula, na sinuosidade das células epidérmicas, e na distribuição e quantidade de fibras no mesofilo evidenciando a interferência das condições de luminosidade nas características morfológicas das microplantas. Essas alterações não prejudicaram o desenvolvimento das microplantas, indicando que não são necessárias etapas de rustificação para a aclimatização deste cultivar.Microprapagated plants usually show difficulties to adapt to ex vitro conditions, and many times are submitted to the rustication process to aim the reduction of all the impacts resulting from the environmental changes. Once the leaf and its annexes are important indicators of adaptability strategies of the plants to adverse environmental conditions, the objective of this work was to compare the leaf anatomy of pineapple cv. IAC "Gomo-de-mel" in vitro cultivated plants with microplants acclimatized in different conditions of luminosity, under mesh, with 50 % of

  20. Occurrence of aflatoxins in peanuts and peanut products determined by liquid chromatography with fluorescence detection

    Directory of Open Access Journals (Sweden)

    Stojanovska-Dimzoska Biljana

    2013-01-01

    Full Text Available Liquid chromatography with fluorescence detection using immunoaffinity column clean-up was a method described for determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2 in peanuts and peanut based products. The validation of the procedure was performed. Good coefficient of correlation was found for all aflatoxins in the range of 0.9993-0.9999. Limit of detection (LOD and limit of quantification (LOQ ranged from 0.003-0.005 mg/kg and 0.009-0.023 mg/kg, respectively, which was acceptable. The mean recovery for total aflatoxins was 88.21%. The method also showed acceptable precision values in the range of 0.171-2.626% at proposed concentration levels for all four aflatoxins. RSDR values (within laboratory reproducibility calculated from the results showed good correlation between two analysts for all aflatoxins and they ranged from 4.93-11.87%. The developed method was applied for the determination of aflatoxins in 27 samples of peanuts and peanut based products. The results showed that 21 peanut samples (77.7% were below LOD of the method. Three samples had positive results over the MRL. There was one extreme value recorded for the total aflatoxins in peanut (289.2 mg/kg and two peanut based products, peanut snack and peanut, with total content of aflatoxins being 16.3 mg/kg and 8.0 mg/kg, respectively. The obtained results demonstrated that the procedure was suitable for the de­termination of aflatoxins in peanuts and peanut based products and it could be implemented for the routine analysis.

  1. Hydroxylapatite chromatography.

    Science.gov (United States)

    Broadhurst, A V

    2001-05-01

    Hydroxylapatite (also called hydroxyapatite), a form of calcium phosphate, can be used as a matrix for the chromatography of both proteins and nucleic acids. Protocols are provided for both standard low-pressure chromatography of a protein mixture using a hydroxylapatite column prepared in the laboratory, and an HPLC method, applicable to proteins and nucleic acids, that uses a commercially available column. Alternate protocols describe column chromatography using a step gradient or batch binding and step-gradient elution.

  2. Studies in the Use of Magnetic Microspheres for Immunoaffinity Extraction of Paralytic Shellfish Poisoning Toxins from Shellfish

    Directory of Open Access Journals (Sweden)

    Christopher Elliott

    2011-01-01

    Full Text Available Paralytic shellfish poisoning (PSP is a potentially fatal human health condition caused by the consumption of shellfish containing high levels of PSP toxins. Toxin extraction from shellfish and from algal cultures for use as standards and analysis by alternative analytical monitoring methods to the mouse bioassay is extensive and laborious. This study investigated whether a selected MAb antibody could be coupled to a novel form of magnetic microsphere (hollow glass magnetic microspheres, brand name Ferrospheres-N and whether these coated microspheres could be utilized in the extraction of low concentrations of the PSP toxin, STX, from potential extraction buffers and spiked mussel extracts. The feasibility of utilizing a mass of 25 mg of Ferrospheres-N, as a simple extraction procedure for STX from spiked sodium acetate buffer, spiked PBS buffer and spiked mussel extracts was determined. The effects of a range of toxin concentrations (20–300 ng/mL, incubation times and temperature on the capability of the immuno-capture of the STX from the spiked mussel extracts were investigated. Finally, the coated microspheres were tested to determine their efficiency at extracting PSP toxins from naturally contaminated mussel samples. Toxin recovery after each experiment was determined by HPLC analysis. This study on using a highly novel immunoaffinity based extraction procedure, using STX as a model, has indicated that it could be a convenient alternative to conventional extraction procedures used in toxin purification prior to sample analysis.

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

    Science.gov (United States)

    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.

  4. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Separation techniques: Chromatography

    Science.gov (United States)

    Coskun, Ozlem

    2016-01-01

    Chromatography is an important biophysical technique that enables the separation, identification, and purification of the components of a mixture for qualitative and quantitative analysis. Proteins can be purified based on characteristics such as size and shape, total charge, hydrophobic groups present on the surface, and binding capacity with the stationary phase. Four separation techniques based on molecular characteristics and interaction type use mechanisms of ion exchange, surface adsorption, partition, and size exclusion. Other chromatography techniques are based on the stationary bed, including column, thin layer, and paper chromatography. Column chromatography is one of the most common methods of protein purification. PMID:28058406

  6. Comprehensive two-dimensional liquid chromatography: Ion chromatography × reversed-phase liquid chromatography for separation of low-molar-mass organic acids

    NARCIS (Netherlands)

    Brudin, S.S.; Shellie, R.A.; Haddad, P.R.; Schoenmakers, P.J.

    2010-01-01

    In the work presented here a novel approach to comprehensive two-dimensional liquid chromatography is evaluated. Ion chromatography is chosen for the first-dimension separation and reversed-phase liquid chromatography is chosen for the second-dimension separation mode. The coupling of these modes is

  7. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  8. Trigo: avaliação tecnológica de novas linhagens Technological evaluation of new lines of wheat

    Directory of Open Access Journals (Sweden)

    Celina Raquel de Oliveira Camargo

    1987-01-01

    Full Text Available Avaliou-se a qualidade tecnológica das linhagens de trigo IAC-22, IAC-31, IAC-37, IAC-41, IAC-46, IAC-57 e IAC-60, obtidas pelo programa de melhoramento do Instituto Agronômico, tomando como controle uma amostra de trigo norte-americano e amostras dos cultivares Alondra-S-46 e IAC-18, comerciais no Estado de São Paulo. Os maiores teores de proteína foram encontrados no 'IAC-22' e nas linhagens IAC-37 e IAC-41, superiores àqueles das farinhas de trigo importado, Alondra-S-46 e IAC-18. Todas as farinhas de trigo apresentaram viscosidade máxima superior a 1.000 unidades amilográficas, indicando a ausência da enzima alfa-amilase. As farinhas de trigo importado e das linhagens IAC-31, IAC-41 e IAC-57 apresentaram características farinográficas típicas de farinha de força média a forte e IAC-18 e IAC-60, de farinha média a fraca. Os extensigramas mostraram que as linhagens IAC-41, IAC-31, IAC-57 e IAC-46 apresentaram glúten com características viscoelásticas adequadas para a produção de pão. Pelo teste de panificação, concluiu-se que as linhagens IAC-31 e IAC-41 produziram pão de qualidade "muito boa", semelhante à da farinha de trigo importado; IAC-57, IAC-37 e IAC-60, pão de qualidade "boa" e similar à do 'Alondra-S-46'; as linhagens IAC-46 e IAC-22 tiveram o pior comportamento em relação à qualidade de pão, "regular", semelhante à do 'IAC-18'.The new wheat lines IAC-22, IAC-31, IAC-37, IAC-41, IAC-46, IAC-57 and IAC-60, obtained from the Wheat Breeding Program of the Instituto Agronômico of the State of São Paulo, Brazil, were submitted to technological tests to evaluate the flour quality. Samples of wheat from the United States and of the wheat cultivars Alondra-S-46 and IAC-18 were used as controls. The wheat flours were submitted to chemical tests to determine the protein, lipid, ash, fiber and carbohidrate composition and to rheologic tests using a farinograph, an extensigraph and a viscoamilograph. The final

  9. Comparative determination of phenytoin by spectrophotometry, gas chromatography, liquid chromatography, enzyme immunoassay, and radioimmunoassay

    International Nuclear Information System (INIS)

    Castro, A.; Ibanez, J.; DiCesare, J.L.; Adams, R.F.; Malkus, H.

    1978-01-01

    Sera from patients being treated with phenytoin were analyzed for the drug by spectrophotometry, gas chromatography, radioimmunoasay, enzyme immunoassay, and liquid chromatography. The assay values obtained were intercompared statistically. Enzyme immunoassay and liquid chromatography appear to be attractive alternatives to the more traditional methods of spectrophotometry and gas chromatography. Our radioimmunoassay data correlated poorly with results by the four other methods

  10. Melhoramento do trigo: XII. Comportamento de novas linhagens e cultivares no Estado de São Paulo Wheat breeding: XII. Evaluation of new inbred lines for the State of São Paulo, Brazil

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo de Oliveira Camargo

    1985-01-01

    Full Text Available Foram comparadas entre si vinte e uma linhagens e quatro cultivares comerciais de trigo através de ensaios instalados em diferentes localidades paulistas, analisando-se os seguintes parâmetros: rendimento de grãos, altura de plantas, ciclo em dias da emergência ao florescimento e da emergência à maturação, porcentagem de plantas acamadas, comprimento da espiga, número de grãos por espiga e por espigueta, número de espiguetas por espiga, peso de cem grãos, resistência à ferrugem do-colmo e da-folha em condições de campo e de casa de vegetação. Em condições de laboratório, foram realizados estudos da tolerância ao alumínio, em soluções nutritivas. Nos ensaios conduzidos em Campinas, em condição de irrigação por aspersão, destacaram-se, quanto à produção de grãos, as linhagens IAC-60 e IAC-67, e, nos de Capão Bonito, IAC-66, IAC-60 e IAC-69 apresentaram maior produtividade. As linhagens IAC-64, IAC-68, IAC-71 e IAC-60 destacaram-se em Tietê, e as linhagens IAC-67, IAC-63 e IAC-64 evidenciaram alta produção de grãos em Maracaí. As linhagens IAC-52, IAC-53, IAC-54, IAC-55, IAC-56, IAC-57, IAC-58, IAC-60, IAC-64, IAC-65, IAC-67, IAC-71 e o 'Alondra-S-46' mostraram plantas de porte semi-anão, diferindo significativamente do 'BH-1146', de porte alto. Em relação à ferrugem-do-colmo (Puccinia graminis f. sp. fruir, as linhagens IAC-62 e IAC-65 e o cultivar Alondra-S-46 foram resistentes às sete raças testadas em estádio de plântula em casa de vegetação e também em condições de campo. Em casa de vegetação, a linhagem IAC-64 foi resistente a quatro raças de P. recondita, agente da ferrugem-da-folha, e IAC-52 e IAC-55, a três raças desse patógeno. Em condição de infecção natural no estádio de planta adulta, as linhagens IAC-51, IAC-56, IAC-61, IAC-62, IAC-63 e IAC-67 apresentaram menor grau de infecção dessa ferrugem, enquanto IAC-51, IAC-60, IAC-63, IAC-68 e IAC-70, bem como 'BH-1146' e 'IAC

  11. Metal-organic frameworks in chromatography.

    Science.gov (United States)

    Yusuf, Kareem; Aqel, Ahmad; ALOthman, Zeid

    2014-06-27

    Metal-organic frameworks (MOFs) emerged approximately two decades ago and are the youngest class of porous materials. Despite their short existence, MOFs are finding applications in a variety of fields because of their outstanding chemical and physical properties. This review article focuses on the applications of MOFs in chromatography, including high-performance liquid chromatography (HPLC), gas chromatography (GC), and other chromatographic techniques. The use of MOFs in chromatography has already had a significant impact; however, the utilisation of MOFs in chromatography is still less common than other applications, and the number of MOF materials explored in chromatography applications is limited. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Recent advances of capillary electrophoresis in pharmaceutical analysis.

    Science.gov (United States)

    Suntornsuk, Leena

    2010-09-01

    This review covers recent advances of capillary electrophoresis (CE) in pharmaceutical analysis. The principle, instrumentation, and conventional modes of CE are briefly discussed. Advances in the different CE techniques (non-aqueous CE, microemulsion electrokinetic chromatography, capillary isotachophoresis, capillary electrochromatography, and immunoaffinity CE), detection techniques (mass spectrometry, light-emitting diode, fluorescence, chemiluminescence, and contactless conductivity), on-line sample pretreatment (flow injection) and chiral separation are described. Applications of CE to assay of active pharmaceutical ingredients (APIs), drug impurity testing, chiral drug separation, and determination of APIs in biological fluids published from 2008 to 2009 are tabulated.

  13. Report: Affinity Chromatography.

    Science.gov (United States)

    Walters, Rodney R.

    1985-01-01

    Supports, affinity ligands, immobilization, elution methods, and a number of applications are among the topics considered in this discussion of affinity chromatography. An outline of the basic principles of affinity chromatography is included. (JN)

  14. Chromatography of phosphorus oxoacids

    International Nuclear Information System (INIS)

    Ohashi, S.

    1975-01-01

    The present state of studies on the chromatographic separation of phosphorus oxoacids is surveyed. In this paper, chromatographic techniques are divided into four groups, i.e. paper and thin-layer chromatography, paper electrophoresis, ion-exchange chromatography, and gel chromatography. The separation mechanisms and characteristics for these chromatographic methods are discussed and some examples for the separation of phosphorus oxoacids are described. As examples of the application of ion-exchange and gel chromatography, studies on the hot atom chemistry of 32 P in solid inorganic phosphates and those on the substitution reactions between diphosphonate (diphosphite) and polyphosphates are reported. (author)

  15. Column Liquid Chromatography.

    Science.gov (United States)

    Majors, Ronald E.; And Others

    1984-01-01

    Reviews literature covering developments of column liquid chromatography during 1982-83. Areas considered include: books and reviews; general theory; columns; instrumentation; detectors; automation and data handling; multidimensional chromatographic and column switching techniques; liquid-solid chromatography; normal bonded-phase, reversed-phase,…

  16. Immune chromatography: a quantitative radioimmunological assay

    International Nuclear Information System (INIS)

    Davis, J.W.; Demetriades, M.; Bowen, J.M.

    1984-01-01

    Immune chromatography, a radioimmunological binding assay, employs paper chromatography to separate immune complexes from free antigen and antibodies. During chromatography free antigen and antibodies become distributed throughout the paper, while immune complexes remain near the bottoms of the strips. The chromatographic differences can be made quantitative by using either iodinated antigens or antibodies. Under these conditions nanogram quantities of antigen can be detected or antibodies in sera diluted several 1000-fold. The immune chromatography assay can also be performed as an indirect assay, since the paper strips are cut from nitrocellulose paper. In this case the immune components are absorbed by the paper during chromatography. Antigen is then detected with an iodinated second antibody. The indirect immune chromatography assay is particularly useful for identifying different sera that react with the same antigen. Reaction with the first serum before chromatography reduces the amount of antigen available to the second serum following chromatography. In addition to characterizing the immune chromatography procedure, we discuss the possible applications of chromatography assays for the quantitation of other types of molecular binding interactions. (Auth.)

  17. Enantioseparations in counter-current chromatography and centrifugal partition chromatography.

    Science.gov (United States)

    Foucault, A P

    2001-01-12

    Examples of chiral separations in counter-current chromatography (CCC) and centrifugal partition chromatography (CPC) are not numerous, due to the difficulty of finding chiral selectors highly selective in the liquid phase as well as a combination of solvents that does not destroy the selectivity and retains the capacity to elute chiral isomers of interest. New ideas and new chiral selectors generally come from other separation techniques, as will be highlighted in this review.

  18. Thin-layer and paper chromatography

    International Nuclear Information System (INIS)

    Sherma, J.

    1986-01-01

    This selective review covers the literature of thin-layer chromatography (TLC) and paper chromatography (PC) cited in Chemical Abstracts from December 5, 1983, through November 25, 1985, and Analytical Abstracts from November 1983 to November 1985. Also researched directly were the following important journals publishing papers on TLC and PC: the Journal of Chromatography (including its bibliography issues), Journal of High Resolution Chromatography and Chromatography Communications, Journal of Chromatographic Science, Chromatographia, Analytical Chemistry, JAOAC, and the special TLC issues of the Journal of Liquid Chromatography. Many of the inherent advantages of TLC that are obvious to workers familiar with high performance, quantitative theory and practice still are not appreciated adequately by the majority of people using chromatography. These include unrestricted access to the separation process; introducing magnetic, thermal, electrical, and other physical forces to improve resolution; high sample throughput; truly multidimensional separations; and the use of controlled multiple gradients. Many advantages of TLC relative to column chromatography were discussed in the Introductions to our 1982 and 1984 reviews of TLC in this Journal. No complete commercial robotics system specifically for TLC has been developed, but all necessary modules are available for such a system. The combination of robotics, with the continued development of theory, practice, and instrumentation will lead eventually to TLC systems that are unrivaled for speed, versatility, accuracy, precision, and sensitivity. 573 references

  19. Rendimento de grãos e qualidade tecnológica de genótipos de trigo em três zonas tritícolas do Estado de São Paulo no biênio 1994-95

    Directory of Open Access Journals (Sweden)

    FELICIO JOÃO CARLOS

    2000-01-01

    Full Text Available Foram avaliados o rendimento de grãos, a estabilidade e adaptabilidade ambiental, a tolerância ao alumínio tóxico e a qualidade tecnológica da farinha de vinte genótipos de trigo em três regiões tritícolas do Estado de São Paulo (Zonas A e B, sequeiro; Zona H, com irrigação por aspersão, no biênio 1994-95. Os resultados mostraram que: (a os genótipos tiveram comportamento regional diferenciado quanto ao rendimento de grãos; (b os genótipos IAC 289, IAC 340 e BR 18 mostraram-se, em média os mais produtivos, não diferindo do 'IAC 304', 'OCEPAR 14', 'IAC 350', 'Panda', 'IAC 60' e 'IAC 348'; (c os genótipos apresentaram, em geral, boa estabilidade produtiva nas diferentes condições ambientais; (d os genótipos IAC 289, IAC 340 e IAC 304 foram responsivos à melhoria ambiental e 'IAC 227', adaptado a ambientes desfavoráveis; (e os genótipos IAC 24, IAC 120, IAC 227, OCEPAR 14, IAC 348, Panda, BR 18, IAC 319, IAC 346, IAPAR 60, IAC 332 e IAC 347 foram tolerantes à toxicidade de Al3+; (f a farinha dos diferentes genótipos apresentou baixa atividade amilásica; (g os genótipos IAC 340, IAC 227, IAC 319 e IAC 60 propiciaram farinha com baixos valores de W (energia de deformação da massa e baixa estabilidade, características próprias de farinha de glúten fraco. Os demais genótipos revelaram característica de glúten forte.

  20. A novel method for radiolabeling antigen-binding receptors of lymphocytes

    International Nuclear Information System (INIS)

    Choi, Y.S.; Lee, M.S.; Rosenspire, A.J.

    1983-01-01

    Antigen-binding receptor (ABR) molecules have been selectively radiolabeled and isolated from immunized chicken spleen cells. The specific radiolabeling of the receptors has been accomplished by utilizing a novel technique employing lactoperoxidase (LPO) covalently linked to antigen (Ag) for which human gammaglobulin was used. The cell surface ABRs were first bound to the Ag-LPO conjugates through specific recognition sites on the Ag portion of the conjugates. The bound LPO portions were then allowed to catalyze the radioiodination of the ABRs. After radiolabeling, cells were solubilized with detergents, ABRs still bound to Ag-LPO conjugates were directly isolated from the lysates via immunoaffinity chromatography utilizing an immunoaffinity reagent directed toward the antigen portion of the ABR-Ag-LPO complex. The radioactive materials were then analyzed via SDS-PAGE under reducing conditions. Most of the specifically-labeled and isolated materials were immunoglobulin (Ig). Both the membrane-bound form of the heavy chain as well as the secreted form were detected, along with the light chain. An additional polypeptide was also selectively labeled and isolated along with the Ig. This may be a molecule closely associated with the membrane immunoglobulin on the B-cell surface. (author)

  1. Simultaneous analysis for water- and fat-soluble vitamins by a novel single chromatography technique unifying supercritical fluid chromatography and liquid chromatography.

    Science.gov (United States)

    Taguchi, Kaori; Fukusaki, Eiichiro; Bamba, Takeshi

    2014-10-03

    Chromatography techniques usually use a single state in the mobile phase, such as liquid, gas, or supercritical fluid. Chromatographers manage one of these techniques for their purpose but are sometimes required to use multiple methods, or even worse, multiple techniques when the target compounds have a wide range of chemical properties. To overcome this challenge, we developed a single method covering a diverse compound range by means of a "unified" chromatography which completely bridges supercritical fluid chromatography and liquid chromatography. In our method, the phase state was continuously changed in the following order; supercritical, subcritical and liquid. Moreover, the gradient of the mobile phase starting at almost 100% CO2 was replaced with 100% methanol at the end completely. As a result, this approach achieved further extension of the polarity range of the mobile phase in a single run, and successfully enabled the simultaneous analysis of fat- and water-soluble vitamins with a wide logP range of -2.11 to 10.12. Furthermore, the 17 vitamins were exceptionally separated in 4min. Our results indicated that the use of dense CO2 and the replacement of CO2 by methanol are practical approaches in unified chromatography covering diverse compounds. Additionally, this is a first report to apply the novel approach to unified chromatography, and can open another door for diverse compound analysis in a single chromatographic technique with single injection, single column and single system. Copyright © 2014. Published by Elsevier B.V.

  2. Expression of human α-fetoprotein in yeast

    International Nuclear Information System (INIS)

    Yamamoto, Ritsu; Sakamoto, Takashi; Nishi, Shinzo; Sakai, Masaharu; Morinaga, Tomonori; Tamaoki, Taiki

    1990-01-01

    Human α-fetoprotein (AFP) was expressed in Saccharomyces cerevisiae, with a plasmid containing the cDNA sequence for human AFP fused with the rat AFP signal peptide. The recombinant AFP was purified from the yeast lysate by DEAE-cellulose and immunoaffinity chromatography. The amino acid composition and the molecular weight of the recombinant AFP were similar to those of hepatoma AFP. N-terminal amino acids sequence analysis indicated that the signal peptide had been processed. The recombinant and hepatoma AFP reacted identically in Ouchterlony immunodiffusion and radioimmunoassay tests. These observations indicated that the yeast recombinant protein had the properties of native AFP

  3. Isolation and characterization of human apolipoprotein M-containing lipoproteins

    DEFF Research Database (Denmark)

    Christoffersen, Christina; Nielsen, Lars Bo; Axler, Olof

    2006-01-01

    Apolipoprotein M (apoM) is a novel apolipoprotein with unknown function. In this study, we established a method for isolating apoM-containing lipoproteins and studied their composition and the effect of apoM on HDL function. ApoM-containing lipoproteins were isolated from human plasma...... with immunoaffinity chromatography and compared with lipoproteins lacking apoM. The apoM-containing lipoproteins were predominantly of HDL size; approximately 5% of the total HDL population contained apoM. Mass spectrometry showed that the apoM-containing lipoproteins also contained apoJ, apoA-I, apoA-II, apoC-I, apo...

  4. INTERAÇÃO ENTRE GENÓTIPOS E AMBIENTE NA PRODUTIVIDADE E NA QUALIDADE TECNOLÓGICA DOS GRÃOS DE TRIGO NO ESTADO DE SÃO PAULO

    Directory of Open Access Journals (Sweden)

    FELÍCIO JOÃO CARLOS

    1998-01-01

    Full Text Available Avaliou-se a influência do ambiente na produtividade e na qualidade tecnológica de dezenove genótipos de trigo, mediante seis experimentos instalados, em condições de sequeiro e de irrigação por aspersão, em 1992, em duas regiões tritícolas paulistas. Destacaram-se para a produtividade de grãos os genótipos IAC 304, IAPAR 60, IAC 303, IAC 313, IAC 350, IAC 332, IAC 306, IAC 309, IAC 297, IAC 324 e IAC 325, na condição de sequeiro, e IAC 312 e IAPAR 60, quando se empregou irrigação. A diferença na produtividade com a irrigação por aspersão foi de 124% na média geral entre os experimentos. As condições climáticas da região de Mococa (SP e o uso da irrigação por aspersão apresentaram tendência de melhorar o peso hectolítrico, o rendimento em farinha, a sedimentação e a energia de deformação da massa (W. Entretanto, não influenciou os parâmetros farinográficos, como percentual de absorção de água, tempo de desenvolvimento da massa e estabilidade. Somente o índice de tolerância à mistura foi influenciado para melhor nessa condição. Os genótipos IAC 24, IAC 287, IAC 353, IAC 297, Anahuac e IAC 311 apresentaram alto valor de estabilidade e IAC 24, IAC 353, IAC 297, Anahuac, IAC 306, IAC 313, IAC 311 e IAC 332, alto valor de W, indicativo da força de panificação. O coeficiente de correlação entre sedimentação (SDS e W apresentou-se significativo, indicando que o método de sedimentação poderia ser utilizado nas primeiras fases de seleção para qualidade.

  5. Influência do ambiente no rendimento e na qualidade de grãos de genótipos de trigo com irrigação por aspersão no Estado de São Paulo Environmental influence on grain yield and grain quality of wheat genotypes with sprinkler irrigation in the State of São paulo, Brazil

    Directory of Open Access Journals (Sweden)

    JOÃO CARLOS FELICIO

    2001-01-01

    Full Text Available Avaliaram-se a influência do ambiente em 20 genótipos de trigo, no rendimento e qualidade de grãos, a adaptabilidade e a reação a doenças, em regiões onde a irrigação se faz necessária para permitir o bom desempenho agronômico de um genótipo. Instalaram-se os experimentos em Tatuí, Votuporanga, Ribeirão Preto e Mococa, Estado de São Paulo, no período de 1995-98. Avaliaram-se, também, a tolerância dos genótipos ao alumínio tóxico em solução nutritiva e a qualidade industrial para panificação. Com bom rendimento de grãos destacaram-se: em Tatuí, os genótipos IAC 351, IAC 335, IAC 289 e Mochis; em Votuporanga, IAC 289, TUI"S" e SERI*3/BUC; em Ribeirão Preto e Mococa, o IAC 370. No conceito de genótipo ideal, o IAC 370 apresentou alta capacidade produtiva, foi responsivo à melhoria do ambiente e sensível às condições desfavoráveis do ambiente. Entre as doenças, a ferrugem-da-folha foi a de abrangência generalizada com maior incidência em Tatuí. Anahuac, IAC 287, CAL/CHKW//VEE"S" e IAC 370 foram os mais suscetíveis ao oídio. Os genótipos Anahuac, IAC 287, JCAM//EMU"S"/YACO"S", PFAU e IAC 339 foram os mais sensíveis à toxicidade por Al3+. Os genótipos Anahuac, IAC 24, IAC 287, IAC 289, IAC 334, PFAU, TUI"S", IAC 339, IAC 370 e IAC 351 apresentaram características de farinha com bom potencial para panificação.Environmental influence was evaluated in 20 wheat genotypes in relation to grain yield and quality, adaptability and disease reaction in regions where irrigation is necessary for good agronomical performance. The experiments were carried out at Tatuí, Votuporanga, Ribeirão Preto, and Mococa in the State of São Paulo, Brazil, during 1995-98. Genotypes were also evaluated for tolerance to aluminum toxicity in nutrient solutions and for industrial quality for bread production. The genotypes IAC 351, IAC 335, IAC 289 and Mochis presented high grain yield in Tatuí; IAC 289, TUI"S" and SERI*3/BUC in

  6. Simultaneous determination of four aflatoxins and ochratoxin A in ginger after inoculation with fungi by ultra-fast liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Yang, Ying; Wen, Jing; Kong, Weijun; Liu, Qiutao; Luo, Hongli; Wang, Jian; Yang, Meihua

    2016-09-01

    Aflatoxins (AFs) and ochratoxin A (OTA) have been detected frequently in food, agricultural products and traditional Chinese medicines, and their presence poses serious health and economic problems worldwide. Ginger can easily be polluted with mycotoxins. In this study, ginger samples were cultivated for 15 days after inoculation with fungi and were prepared based on ultrasound-assisted solid-liquid extraction using methanol/water followed by immunoaffinity column clean-up and analysed by ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) for AFs and OTA. The limits of detection and quantification of AFs and OTA were 0.04-0.30 µg mL(-1) and 0.125-1.0 µg mL(-1) , respectively. The recoveries were 82.0-100.2%. After 15 days' cultivation, no macroscopic mildew was found in ginger. But, the content of AFB1 expressed an increasing trend in ginger, peel [less than the limit of quantification (LOQ)] to the innermost layer (51.86 µ mL(-1) ), AFB2 was only detected in the innermost layer at the level of 0.87 µ mL(-1) . A small amount (

  7. Resistência de soja a insetos: IV. Comportamento de cultivares e linhagens em relação a Hedilepta indicata (Fabr. Resistance of soybean to insects: IV. Performance of cultivars and lines in relation to Hedilepta indicata (Fabr.

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenção

    1985-01-01

    Full Text Available Em condições de campo e de telado, estudou-se o comportamento das seguintes linhagens e cultivares de soja em relação à lagarta-enroladeira, Hedilepta indicata (Fabr., 1775: PI 227687, IAC 73-228, IAC 79-1823, 'Santa Rosa', IAC 80-596-2, 'IAC 12', 'IAC 8', IAC 78-2318, D 72-9601-1, PI 171451, 'IAC São Carlos' e PI 229358, quanto ao número de pontos de ataque do inseto. Tanto no campo como em telado, IAC 73-228 e PI 229358 apresentaram, respectivamente, o menor e o maior valor. Em condições de campo, PI 227687 e IAC 73-228 sofreram as menores perdas de área foliar devidas ao ataque de H. indicata, enquanto 'IAC São Carlos', PI 171451 e PI 229358 se mostraram como os mais suscetíveis. Em outro experimento conduzido em campo, utilizando-se PI 274454, PI 274453, IAC 73-228, 'IAC 12', IAC 80-596-2, 'UFV-1', IAC 78-2318 e 'Paraná', os dois primeiros apresentaram alto nível de resistência ao inseto, superior ao exibido por IAC 73-228, sendo que 'Paraná' teve a maior perda de área foliar. Ainda em condições de campo, em área de seleção de plantas F2 descendentes do cruzamento de 'Paraná' com PI 274453, foram avaliadas, individualmente, plantas quanto à área foliar comida: os resultados obtidos sugerem que a resistência da PI 274453 a H. indicata seja devida a um gene dominante.Performance of soybean cultivars and lines in relation to H. indicata was studied under field and screen house conditions. Differences in the number of points of attack (characterized by the rolling or junction of the folioles by means of silk secretion were evaluated in PI 227687, IAC 73-228, IAC 79-1823, 'Santa Rosa', IAC 80-596-2, 'IAC 12', 'IAC 8', IAC 78-2318, D 72-9601-1, PI 171451, 'IAC São Carlos' and PI 229358; in both, field and screen house conditions, IAC 73-228 and PI 229358 showed, respectively, the lowest and the highest values. In the field, PI 227687 and IAC 73-228 presented low defoliation, while 'IAC São Carlos', PI 171451 and PI

  8. Tolerância de cultivares de arroz a diferentes níveis de alumínio em solução nutritiva Rice cultivars tolerance to different levels of aluminum in nutrient solution

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo de Oliveira Camargo

    1983-01-01

    Full Text Available Em condições controladas de crescimento, foram estudados 22 cultivares de arroz, em soluções nutritivas com temperaturas de 25 ± 1°C e 30 ± 1°C, com cinco diferentes níveis de alumínio, em recipientes de 8,3 litros com 330 plântulas por recipiente. A tolerância foi medida pela capacidade de as raízes primárias continuar a crescer, em solução sem alumínio, após um período de 72 horas em solução contendo uma concentração conhecida de alumínio. Nas soluções nutritivas com temperatura de 25 ± 1°C, os cultivares IAC-899 e IR-841 foram sensíveis a 10mg/litro de Al3+; IR-43, IR-45 e IR-8, foram sensíveis a 20mg/litro de Al3+; CICA-4 e IR-42, a 40mg/litro de Al3+, e IAC-435, IAC-164, Pérola, Batatais, Pratão Precoce, Blue Bonnet, IAC-120, IAC-47, IAC-1246, IAC-25, IAC-165, Pratão, Dourado Precoce e CICA-8 foram tolerantes a 40mg/litro de Al3+. Quando foram utilizadas soluções nutritivas com temperatura de 30 ± 1°C, todos os cultivares de arroz estudados apresentaram melhor desenvolvimento radicular do que a 25 ± 1°C e se mostraram tolerantes a 5, 10 e 20mg/litro de Al3+. Com a concentração de 40mg/litro de Al3+, os cultivares Dourado Precoce, CICA-4, IR-42, IR-43, IR-45, IR-8, IAC-899, IR-665-4-5-5 e IR-841 foram sensíveis; IAC-47, Blue Bonnet, IAC-1246, IAC-164, Pratão, Pratão Precoce, CICA-8, IAC-435, IAC-120, IAC-25, IAC-165, Pérola e Batatais, tolerantes. A presença do alumínio nas soluções nutritivas foi prejudicial a todos os cultivares tolerantes e sensíveis. Os dados obtidos permitiram classificar os cultivares estudados nas seguintes classes de tolerância ao alumínio: tolerantes: IAC-435, IAC-120, IAC-47, IAC-1246, IAC-25, IAC-165, IAC-164, Pérola, Batatais, Pratão Precoce, Blue Bonnet; moderadamente tolerantes: Pratão, Dourado Precoce e CICA-8, e sensíveis: CICA-4, IR-42, IR-43, IR-45, IR-8, IAC-899, IR-665-4-5-5 e IR-841.Twenty two rice cultivars were studied in nutrient solution in

  9. Liquid Chromatography in 1982.

    Science.gov (United States)

    Freeman, David H.

    1982-01-01

    Reviews trends in liquid chromatography including apparatus, factors affecting efficient separation of a mixture (peak sharpness and speed), simplified problem-solving, adsorption, bonded phase chromatography, ion selectivity, and size exclusion. The current trend is to control chemical selectivity by the liquid phase. (Author/JN)

  10. Resistência de plantas de coffea arabica, coffea canephora e híbridos interespecíficos à cercosporiose

    Directory of Open Access Journals (Sweden)

    Flávia Rodrigues Alves Patricio

    2010-12-01

    Full Text Available O presente estudo objetivou avaliar a resistência de plantas de Coffea arabica, C. canephora e de híbridos interespecíficos, à cercosporiose (Cercospora coffeicola, importante doença da cultura do cafeeiro. Foram realizados dois experimentos em 2003, em Campinas (SP, com mudas das cultivares de C. arabica, Mundo Novo IAC 388-17-1, Mundo Novo IAC 376-4, Bourbon Amarelo, Bourbon Vermelho, Obatã IAC 1669-20, Catuaí Vermelho IAC 144, Catuaí Amarelo IAC 62, Icatu Precoce IAC 3282, Icatu Vermelho IAC 4045, Ouro Verde IAC H5010-5 e Tupi IAC 1669-33; de C. canephora, Robusta IAC 1653-7 e Apoatã IAC 2258, além de dois híbridos interespecíficos Piatã IAC 387 e Híbrido de Timor IAC 1559-13. As mudas foram submetidas à inoculação com uma suspensão de conídios preparada com cinco isolados coletados em diferentes regiões do Estado de São Paulo. Os materiais mais suscetíveis foram Robusta IAC 1653-7, Apoatã IAC 2258, Híbrido de Timor IAC 1559-13, Bourbon Vermelho e Bourbon Amarelo com incidência entre 63,1% e 81,6% no primeiro experimento e entre 70% e 93,3% no segundo e severidade (notas 1-6 entre 2,92 e 3,42 no primeiro experimento e entre 3,64 e 2,79 no segundo. Os materiais mais resistentes foram Piatã IAC 387, Ouro Verde IAC H5010-5 e Tupi IAC 1669-33, com incidência entre 28,4% e 35,5% no primeiro experimento e 21,1% e 55,6% no segundo, e severidade entre 1,44 e 1,73 e entre 1,28 e 1,88, respectivamente, no primeiro e segundo experimentos.

  11. Variability of soybean germplasm in relation to phosphorus uptake and use efficiency Variabilidade em germoplasma de soja para eficiência na absorção e utilização de fósforo

    Directory of Open Access Journals (Sweden)

    Ângela Maria Cangiani Furlani

    2002-09-01

    Full Text Available Plant efficiency for phosphorus uptake and utilization may contribute to improve crop yield potential in situations of low P availability. Twenty nine soybean [Glycine max (L. Merr.] cultivars were evaluated and classified in relation to the response to phosphorus (P levels in nutrient solution. P uptake and use efficiency were estimated by the variables: shoot and root dry matter (DM yield, P-concentrations and contents in plant parts and P-efficiency index (EI. The experiment was conducted in a greenhouse, during 1999, at Campinas, State of São Paulo, Brazil. The experimental design consisted of randomized complete blocks, arranged in split-plots, with three replications. The main plots were the P levels in the nutrient solution (64.5; 129; 258 and 516 mmol L-1, and the subplots were the twenty-nine soybean cultivars, grouped according days to maturity. The plants were harvested at flowering, separated in shoots and roots for dry matter determination and chemical analysis. The analyses of variance indicated differences in plant responses to P-levels and cultivars. Multivariate analysis showed high correlation among the variables shoot-DM, total-DM and shoot P-concentration and P-efficiency index (EI. Cultivars were classified in efficient-responsive (ER-- 'IAC-1', 'IAC-2', 'IAC-4', 'IAC-5', 'IAC-6', 'IAC-9', 'Sta. Rosa' and 'UFV-1'; efficient-non-responsive (ENR -- 'IAC-7', 'IAC-11', 'IAC-15', 'S. Carlos' and 'Cristalina'; inefficient-responsive (IR -- 'IAC-8', 'IAC-10', 'IAC-14', 'Bossier' and 'Foscarin'; and inefficient-non-responsive (INR -- 'IAC-12', 'IAC-13', 'IAC-16', 'IAC-17', 'IAC-18', 'IAC-19', 'IAC-20', 'IAC-22', 'Paraná', 'IAS-5' and 'BR-4'. The efficient-responsive soybean cultivars showed the highest values for shoot and total DM and EI, and the lowest shoot P-concentrations.A eficiência da planta na absorção e utilização de fósforo em situação de baixa disponibilidade do nutriente pode contribuir para aumentar o

  12. Application of gas chromatography in hydrogen isotope separation

    International Nuclear Information System (INIS)

    Ye Xiaoqiu; Sang Ge; Peng Lixia; Xue Yan; Cao Wei

    2008-01-01

    The principle of gas chromatographic separation of hydrogen isotopes was briefly introduced. The main technology and their development of separating hydrogen isotopes, including elution chromatography, hydrogen-displacement chromatography, self-displacement chromatography and frontal chromatography were discussed in detail. The prospect of hydrogen isotope separation by gas chromatography was presented. (authors)

  13. Determination of radiochemical purity using gas chromatography

    International Nuclear Information System (INIS)

    1975-01-01

    The concepts of chromatography, gas chromatography, activity, radiochemical impurity are defined; the procedure of the application of gas chromatography for detecting radiochemical purity of substances is standardized. (E.F.)

  14. Human epidermal growth factor: molecular forms and application of radioimmunoassay and radioreceptor assay

    International Nuclear Information System (INIS)

    Hirata, Y.; Orth, D.N.

    1981-01-01

    Epidermal growth factor (EGF), a 53 amino acid polypeptide, was first isolated by Cohen. EGF's growth-promoting activity is not limited to epidermal cells, but is expressed on a wide variety of tissues derived from a number of different species. Human EGF (hEGF) was isolated and subsequently purified from human urine. Unexpectedly, a close structural relationship was recognized between mEGF and human β-urogastrone. The authors recently developed both an homologous hEGF radioimmunoassay (RIA) and a radioreceptor assay (RRA) using a human placental membrane fraction. Using these assays, the molecular size of hEGF in human body fluids and tissues was evaluated, and partial characterization of a high molecular weight form of hEGF isolated from human urine was carried out. The concentrations of immunoreactive hEGF were also determined in human tissues and plasma after extraction either with cationic exchange chromatography or with immunoaffinity chromatography. (Auth.)

  15. The weight of flash chromatography: A tool to predict its mass intensity from thin-layer chromatography

    Directory of Open Access Journals (Sweden)

    Freddy Pessel

    2016-11-01

    Full Text Available Purification by flash chromatography strongly impacts the greenness of a process. Unfortunately, due to the lack of the relevant literature data, very often this impact cannot be assessed thus preventing the comparison of the environmental factors affecting the syntheses. We developed a simple mathematical approach to evaluate the minimum mass intensity of flash chromatography from the retention factor values determined by thin-layer chromatography.

  16. Supercritical fluid chromatography

    Science.gov (United States)

    Vigdergauz, M. S.; Lobachev, A. L.; Lobacheva, I. V.; Platonov, I. A.

    1992-03-01

    The characteristic features of supercritical fluid chromatography (SCFC) are examined and there is a brief historical note concerning the development of the method. Information concerning the use of supercritical fluid chromatography in the analysis of objects of different nature is presented in the form of a table. The roles of the mobile and stationary phases in the separation process and the characteristic features of the apparatus and of the use of the method in physicochemical research are discussed. The bibliography includes 364 references.

  17. Comprehensive two-dimensional liquid chromatography and hyphenated liquid chromatography to study the degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, T.

    2005-01-01

    Size exclusion chromatography (SEC), gradient polymer elution chromatography (GPEC) and liquid chromatography at critical conditions (LC-CC) have been developed and applied to observe chemical changes in poly(bisphenol A)carbonate (PC) due to hydrolytic degradation. Especially LC-CC appeared to be

  18. Characterisation of uremic "Middle molecular"fractions by gas chromatography mass spectrometry, isotachophoresis, and liquid chromatography

    NARCIS (Netherlands)

    Schoots, A.C.; Mikkers, F.E.P.; Claessens, H.A.; Smet, de R.; Landschoot, van N.; Ringoir, S.M.G.

    1982-01-01

    Uremic ultrafiltrates (and normal serum, for comparison) were fractionated by means of gel filtration. The collected fractions were further investigated by combined analytical techniques: "high- performance" liquid chromatography, gas chromatography, mass spectrometry, and isotachophoresis.

  19. Thin-Layer and Paper Chromatography.

    Science.gov (United States)

    Sherma, Joseph; Fried, Bernard

    1984-01-01

    Reviews literature on chromatography examining: books, reviews, student experiments; chromatographic systems, techniques, apparatus; detecting and identification of separated zones; preparative chromatography and radiochromatography; and applications related to specific materials (such as acids, alcohols, amino acids, antibiotics, enzymes, dyes,…

  20. Capillary gas-solid chromatography

    International Nuclear Information System (INIS)

    Berezkin, V.G.

    1996-01-01

    Modern state of gas adsorption chromatography in open capillary columns has been analyzed. The history of the method development and its role in gas chromatography, ways to construct open adsorptional capillary columns, foundations of the theory of retention and washing of chromatographic regions in gas adsorption capillary columns have been considered. The fields is extensively and for analyzing volatile compounds of different isotopic composition, inorganic and organic gases, volatile organic polar compounds, aqueous solutions of organic compounds. Separation of nuclear-spin isomers and isotopes of hydrogen is the first illustrative example of practical application of the adsorption capillary chromatography. It is shown that duration of protium and deuterium nuclear isomers may be reduced if the column temperature is brought to 47 K

  1. Produção e vigor da videira 'Niágara Rosada' relacionados com o porta-enxerto Yield and plant vigor of 'Niágara Rosada' grape vine related to the rootstock

    Directory of Open Access Journals (Sweden)

    Dário Pauletto

    2001-01-01

    Full Text Available Avaliou-se a produção e o vigor da videira 'Niágara Rosada' sobre os porta-enxertos 'IAC 313', 'IAC 766', 'Kober 5BB', 'Traviú'(106-8 Mgt e 'Schwarzmann', no período de 1990 a 1998, em Taubaté,SP. As maiores produções médias foram obtidas quando se utilizaram os porta enxertos 'IAC 313' e 'IAC 766', totalizando 2,69 kg/planta e 2,59 kg/planta, respectivamente. As produções alcançadas com os porta-enxertos 'Kober5BB' e 'Schwarzmann' foram, em média, 110% menores que os anteriores, enquanto o 'Traviú' apresentou comportamento intermediário. Os porta-enxertos 'IAC 313' e 'IAC 766' também induziram maior vigor à copa, representado pela maior massa de ramos podados e maior diâmetro das plantas. Para a formação de um vinhedo com 'Niágara Rosada', recomenda-se, para a região, os porta-enxertos 'IAC 313', 'IAC 766' ou 'Traviú'.The yield and plant vigor of 'Niágara Rosada' grafted on the 'IAC 313', 'IAC 766', 'Kober 5BB', 'Traviú' (106-8 Mgt and 'Schwarzmann' rootstocks were evaluated from 1990 to 1998, in Taubaté,SP, Brazil. The highest average yields were obtained on the 'IAC 313' and 'IAC 766' rootstocks, reaching 2.69 kg/plant and 2.59 kg/plant, respectively. Yields on 'Kober 5BB' and 'Schwarzmann' were 110% smaller than on the previous ones, while 'Traviú' showed intermediary behavior. 'IAC 313' and 'IAC 766' also induced higher vigor in the vine, represented by higher mass of pruned branches and higher diameter of plant. 'Niágara Rosada' cultivation in the region is recommended on the 'IAC 313', 'IAC 766' or 'Traviú' rootstocks.

  2. Effects of muffin processing on fumonisins from 14C-labeled toxins produced in cultured corn kernels.

    Science.gov (United States)

    Avantaggiato, Giuseppina; De La Campa, Regina; Miller, J David; Visconti, Angelo

    2003-10-01

    The persistence of fumonisins during cooking is known to be affected by several factors, including thermal degradation and the presence of various ingredients in corn-based food recipes that can react with the toxin. A method for the production of corn kernels containing 14C-fumonisins was developed. The corn kernels were colonized by Fusarium verticillioides MRC 826 and supplemented with 1,2-14C-sodium acetate. The specific activity of 14C-FB1 produced made the study of its fate in cornmeal muffins possible. The double-extraction acetonitrile-water-methanol/immunoaffinity column/o-phthaldialdehyde high-performance liquid chromatography (HPLC) method was used to determine FB1 levels in cornmeal muffins. Reductions in FB1 levels in muffins spiked with 14C-labeled and unlabeled FB1 (43 and 48%, respectively) were similar, indicating that the extraction method was efficient and consistent with previous reports. However, with the labeled corn kernel material, recovery levels based on the 14C counts for the eluate from an immunoaffinity column were much higher (90%). This finding indicates that some fumonisin-related compounds other than FB1 that were present in the cornmeal were recognized by the antibodies but not by the HPLC method.

  3. Large scale chromatographic separations using continuous displacement chromatography (CDC)

    International Nuclear Information System (INIS)

    Taniguchi, V.T.; Doty, A.W.; Byers, C.H.

    1988-01-01

    A process for large scale chromatographic separations using a continuous chromatography technique is described. The process combines the advantages of large scale batch fixed column displacement chromatography with conventional analytical or elution continuous annular chromatography (CAC) to enable large scale displacement chromatography to be performed on a continuous basis (CDC). Such large scale, continuous displacement chromatography separations have not been reported in the literature. The process is demonstrated with the ion exchange separation of a binary lanthanide (Nd/Pr) mixture. The process is, however, applicable to any displacement chromatography separation that can be performed using conventional batch, fixed column chromatography

  4. Populações de milho: características agronômicas e tecnológicas Maize populations performance as to agronomic and technological characteristics

    Directory of Open Access Journals (Sweden)

    Marlene Lima

    1988-01-01

    Full Text Available Avaliaram-se duas populações de milho de grãos brancos (IAC-Taitinga e IAC-Moroti e duas de grãos amarelos (IAC-Taiúba e IAC-Iubatã e os cruzamentos recíprocos entre as de grãos brancos e três testemunhas (Ag-401, C-601 e IAC-Porangatu, em dois locais, quanto a características agronômicas. Com exceção das testemunhas, testaram-se também tais populações quanto aos principais parâmetros de interesse tecnológico, relacionados com o rendimento e qualidade do fubá mimoso, para uso em panificação. Foram observadas diferenças altamente significativas entre os tratamentos para os caracteres produtividade de grãos, altura da planta e de inserção da espiga, rendimento de gérmen e de fubá mimoso, volume específico comparativo (V.E.C. e escore total comparativo (Es. T.C.. As populações, de modo geral, apresentaram altos níveis de produção de grãos, sendo o maior valor obtido pela população IAC-Taitinga. Sete dos materiais estudados apresentaram porte médio e dois, porte baixo. A população IAC Taitinga, sem diferir de IAC-Moroti e do híbrido IAC-Taitinga x IAC Moroti, apresentou o maior valor para rendimento de fubá mimoso. A IAC-Taiúba sobressaiu-se das demais quanto ao V.E.C. e só não alcançou valor máximo para Es.T.C. devido à cor amarela dos grãos. A IAC-Taitinga e o híbrido IAC-Taitinga x IAC-Moroti mostraram valores iguais ao padrão (100% para Es.T.C. Foi observado efeito maternal atuando no rendimento do fubá mimoso obtido.White and yellow grained maize populations and some of their reciprocal crosses were evaluated as to several agronomic traits as well as to flour yield and bread characteristics. Some populations, including the hybrids under testing showed high grain yield potentials, at the same levels of commercial hybrids Ag-401 e C-601. Significant differences were recorded for plant and ear height, among the entries studied. 'IAC-Taitinga', without differing- from 'IAC-Moroti' and 'IAC

  5. FRAÇÕES PROTÉICAS E GLOBULINA PRINCIPAL DE GRÃO-DE-BICO (CICER ARIETINUM L., CV IAC-MARROCOS

    Directory of Open Access Journals (Sweden)

    Maraiza Aparecida SILVA

    2009-07-01

    Full Text Available

    O objetivo deste trabalho foi determinar a composição química, as características de solubilidade da fração protéica e isolar a globulina principal do grão-de-bico cultivar IAC-Marrocos. A farinha do grão-de-bico descorticada apresentou 23,99% de proteína, 10,9% de umidade, 2.73% de cinzas, 8,6% de extrato etéreo e 1,05% de fibra. A solubilidade das proteínas da farinha mostrou-se dependente das condições de extração, tais corno tipo e concentração de sal. tempo e pH. O aquecimento a 121,1 °C/15 minutos reduziu a solubilidade, independente da concentração salina e pH. A extração fracionada e seqüencial das proteínas da farinha em diferentes solventes mostrou que 83% da proteína total foi solubilizada, a fração protéica majoritária é a globulina com 41.79% do total, seguida da albumina 16,18%, glutelina 9,99% e prolamina 0,48%. A globulina principal foi isolada e submetida à cromatografia de filtração em gel e de troca iônica. A fração principal apresentou elevado grau de homogeneidade, com apenas uma banda de proteína presente na eletroforese em gel de poliacrilamida e seu peso molecular com base em cromatografia de filtração em Sephadex G-200 foi estimado em 325.000 daltons e apresentou também um teor de glícides de 0,90% .

  6. Overview of online two-dimensional liquid chromatography based on cell membrane chromatography for screening target components from traditional Chinese medicines.

    Science.gov (United States)

    Muhammad, Saqib; Han, Shengli; Xie, Xiaoyu; Wang, Sicen; Aziz, Muhammad Majid

    2017-01-01

    Cell membrane chromatography is a simple, specific, and time-saving technique for studying drug-receptor interactions, screening of active components from complex mixtures, and quality control of traditional Chinese medicines. However, the short column life, low sensitivity, low column efficiency (so cannot resolve satisfactorily mixture of compounds), low peak capacity, and inefficient in structure identification were bottleneck in its application. Combinations of cell membrane chromatography with multidimensional chromatography such as two-dimensional liquid chromatography and high sensitivity detectors like mass have significantly reduced many of the above-mentioned shortcomings. This paper provides an overview of the current advances in online two-dimensional-based cell membrane chromatography for screening target components from traditional Chinese medicines with particular emphasis on the instrumentation, preparation of cell membrane stationary phase, advantages, and disadvantages compared to alternative approaches. The last section of the review summarizes the applications of the online two-dimensional high-performance liquid chromatography based cell membrane chromatography reported since its emergence to date (2010-June 2016). © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Endoscopically Assisted Drilling, Exposure of the Fundus through a Presigmoid Retrolabyrinthine Approach: A Cadaveric Feasibility Study.

    Science.gov (United States)

    Muelleman, Thomas; Shew, Matthew; Alvi, Sameer; Shah, Kushal; Staecker, Hinrich; Chamoun, Roukouz; Lin, James

    2018-01-01

    The presigmoid retrolabyrinthine approach to the cerebellopontine angle is traditionally described to not provide access to the internal auditory canal (IAC). We aimed to evaluate the extent of the IAC that could be exposed with endoscopically assisted drilling and to measure the percentage of the IAC that could be visualized with the microscope and various endoscopes after drilling had been completed. Presigmoid retrolabyrinthine approaches were performed bilaterally on 4 fresh cadaveric heads. We performed endoscopically assisted drilling to expose the fundus of the IAC, which resulted in exposure of the entire IAC in 8 of 8 temporal bone specimens. The microscope afforded a mean view of 83% (n = 8) of the IAC. The 0°, 30°, 45°, and 70° endoscope each afforded a view of 100% of the IAC in 8 of 8 temporal bone specimens. In conclusion, endoscopic drilling of the IAC of can provide an extradural means of exposing the entire length of the IAC while preserving the labyrinth.

  8. Melhoramento do limoeiro-taiti por seleção de clones Tahiti lime breeding through clonal selection

    Directory of Open Access Journals (Sweden)

    J. O. Figueiredo

    1976-01-01

    Full Text Available Neste trabalho são relatados os resultados de produção e vigor das plantas em um experimento de competição de seis clones de limoeiro-taiti (Citrus latifolia Tanaka enxertados no porta-enxerto limoeiro-cravo (Citrus limonia Osbeck. Os resultados de seis anos consecutivos mostraram que o clone IAC 5 foi o mais produtivo superando, em média, todos os outros nas colheitas de janeiro, julho e outubro. Em segundo lugar colocou-se o IAC 2, cuja produção máxima se localizou, porém, no mês de abril, quando os preços do mercado são os mais baixos. O IAC 6 foi inferior a todos. Os clones IAC 1, IAC 3 e IAC 4, comportaram-se de maneira intermediária e a distribuição da produção do IAC 1 foi a mais favorável. O clone IAC 5 foi também o mais vigoroso e não apresentou fissuras na casca do tronco e dos ramos. IAC 2 foi o clone de menor vigor e juntamente com IAC 1 e IAC 6, o mais suscetível à incidência de fissuras.Six selected clones of Tahiti lime (Citrus latifolia Tanaka were evaluated in a field trial at the Estação Experimental de Limeira for fruit production and plant vigor, during six consecutive years. All six clones had the Rangpur lime (Citrus limonia Osbeck as rootstock. The relationship between monthly fruit price and seasonal yield data was also investigated. The clone IAC 5 showed the highest yield in January, July, and October when Tahiti lime price is maximum. This selection had the most vigorous plants with absence of cracks in the bark of the trunk and branches. The least vigorous material was the IAC 2 selection with a top yield in April, when fruit price is minimum. The clones IAC 1, IAC 3, and IAC 4 showed intermediate production while IAC 6 revealed the lowest yield.

  9. Analysis of radioactive mixed hazardous waste using derivatization gas chromatography/mass spectrometry, liquid chromatography, and liquid chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Campbell, J.A.; Lerner, B.D.; Bean, R.M.; Grant, K.E.; Lucke, R.B.; Mong, G.M.; Clauss, S.A.

    1994-08-01

    Six samples of core segments from Tank 101-SY were analyzed for chelators, chelator fragments, and several carboxylic acids by derivatization gas chromatography/mass spectrometry. The major components detected were ethylenediaminetetraacetic acid, nitroso-iminodiacetic acid, nitrilotriacetic acid, citric acid, succinic acid, and ethylenediaminetriacetic acid. The chelator of highest concentration was ethylenediaminetetraacetic acid in all six samples analyzed. Liquid chromatography was used to quantitate low molecular weight acids including oxalic, formic, glycolic, and acetic acids, which are present in the waste as acid salts. From 23 to 61% of the total organic carbon in the samples analyzed was accounted for by these acids

  10. Resistência de soja a insetos: VII. Avaliação de danos de percevejos em cultivares e linhagens Resistance of soybean to insects: VII. Evaluation of damage to cultivars and lines by stink bugs

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenção

    1987-01-01

    Full Text Available Em dois anos consecutivos (1980/81 e 1981/82 estudou-se, em Campinas, o comportamento de oito linhagens (IAC 73-228, IAC 77-3802, IAC 77-3823, IAC 78-2296, IAC 78-2318, IAC 78-3258, IAC 78-3278 e D72-9601-1 e dois cultivares (Santa Rosa e TMU de soja em relação ao ataque de percevejos em campo. No primeiro ano, a infestação natural de Nezara viridula (L e Piezodorus guildinii (West. foi complementada com liberação de adultos de Euschistus heros (Fabr. coletados em lavouras de soja. No segundo ano, não houve necessidade de infestações artificiais, já que as populações naturais de N. viridula e P. guildinii estavam altas. Como critérios para avaliação de dano, usaram-se: retenção foliar, produção de grãos, produção dividida em quatro classes de dano, porcentagem em peso de grãos danificados, peso de cem sementes, teor de óleo e poder germinativo. IAC 73-228 e IAC 78-2318 comportaram-se como os mais resistentes.During the seasons of 1980/81 and 1981/82, the performance of eight soybean lines (IAC 73-228, IAC 77-3802, IAC 77-3823, IAC 78-2296, IAC 78-2318, IAC 78-3258, IAC 78-3278 and D72-9601-1 and two cultivars (Santa Rosa and TMU was evaluated in relation to the attack of stink bugs in the field, at Campinas, State of São Paulo, Brazil. In the season of 1980/81, the low natural infestation of Piezodorus guildinii (West. and Nezara viridula (L. was supplemented by liberation of Euschistus heros (Fabr. adults collected on soybean crops; in the following season, the high natural infestation was sufficient to cause severe damage to soybeans. Seven criteria of damage evaluation were utilized: foliar retention, yield, yield divided in four damage classes, percentage of the damage grain weight, weight of hundred seeds, oil content and germination percentage. The line IAC 73-228 confirmed its resistance and the same performance was observed for the IAC 78-2318. Nevertheless, both these lines have as unfavourable characteristics

  11. Gas chromatography in space

    Science.gov (United States)

    Akapo, S. O.; Dimandja, J. M.; Kojiro, D. R.; Valentin, J. R.; Carle, G. C.

    1999-01-01

    Gas chromatography has proven to be a very useful analytical technique for in situ analysis of extraterrestrial environments as demonstrated by its successful operation on spacecraft missions to Mars and Venus. The technique is also one of the six scientific instruments aboard the Huygens probe to explore Titan's atmosphere and surface. A review of gas chromatography in previous space missions and some recent developments in the current environment of fiscal constraints and payload size limitations are presented.

  12. Counter-current motion in counter-current chromatography.

    Science.gov (United States)

    Ito, Yoichiro

    2014-12-12

    After the CCC2012 meeting, I have received an e-mail regarding the terminology of "Countercurrent Chromatography". It stated that the term "Countercurrent" is a misnomer, because its stationary phase is motionless in the column and that the method should be renamed as liquid-liquid separations or centrifugal separations. However, it was found that these names are already used for various other techniques as found via Google search. The term "Countercurrent Chromatography" was originally made after two preparative methods of Countercurrent distribution and liquid Chromatography, both having no countercurrent motion in the column. However, it is surprising to find that this F1 hybrid method "Countercurrent Chromatography" can clearly exhibit countercurrent motion within the separation column in both hydrodynamic and hydrostatic equilibrium systems. This justifies that "Countercurrent Chromatography" is a proper term for this chromatographic method. Published by Elsevier B.V.

  13. Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

    International Nuclear Information System (INIS)

    Shu, Xikai; Wang, Mei; Liu, Daicheng; Wang, Daijie; Lin, Xiaojing; Liu, Jianhua; Wang, Xiao; Huang, Luqi

    2013-01-01

    An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-β-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-β-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR). (author)

  14. Preparative separation of polyphenols from artichoke by polyamide column chromatography and high-speed counter-current chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Shu, Xikai; Wang, Mei; Liu, Daicheng [College of Life Science, Shandong Normal University, Jinan, Shandong (China); Wang, Daijie; Lin, Xiaojing; Liu, Jianhua; Wang, Xiao; Huang, Luqi, E-mail: wxjn1998@126.com [Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan, Shandong (China)

    2013-09-01

    An efficient method for the rapid separation and purification of polyphenols from artichoke by polyamide column chromatography in combination with high-speed counter-current chromatography (HSCCC) was successfully built. The crude ethanol extracts from dry artichoke were first pre-separated by polyamide column chromatography and divided in two parts as sample 1 and sample 2. Then, the samples were further separated by HSCCC and yielded 7.8 mg of chlorogenic acid (compound I), 24.5 mg of luteolin-7-O-{beta}-D-rutinoside (compound II), 18.4 mg of luteolin-7-O-{beta}-D-glucoside (compound III), and 33.4 mg of cynarin (compound IV) with purity levels of 92.0%, 98.2%, 98.5%, and 98.0%, respectively, as determined by high-performance liquid chromatography (HPLC) method. The chemical structures of these compounds were identified by electrospray ionization-mass spectrometry (ESI-MS) and nuclear magnetic resonance (NMR). (author)

  15. Micellar liquid chromatography

    International Nuclear Information System (INIS)

    Basova, Elena M; Ivanov, Vadim M; Shpigun, Oleg A

    1999-01-01

    Background and possibilities of practical applications of micellar liquid chromatography (MLC) are considered. Various retention models in MLC, the effects of the nature and concentration of surfactants and organic modifiers, pH, temperature and ionic strength on the MLC efficiency and selectivity are discussed. The advantages and limitations of MLC are demonstrated. The performance of MLC is critically evaluated in relationship to the reversed-phase HPLC and ion-pair chromatography. The potential of application of MLC for the analysis of pharmaceuticals including that in biological fluids and separation of inorganic anions, transition metal cations, metal chelates and heteropoly compounds is described. The bibliography includes 146 references.

  16. Analysis of zearalenone and α-zearalenol in 100 foods and medicinal plants determined by HPLC-FLD and positive confirmation by LC-MS-MS.

    Science.gov (United States)

    Kong, Wei-Jun; Shen, Hong-Hong; Zhang, Xiao-Fei; Yang, Xiao-Li; Qiu, Feng; Ou-yang, Zhen; Yang, Mei-Hua

    2013-05-01

    Mycotoxins, which may contaminate many foods and medicinal plants, are poisonous to humans. A high-performance liquid chromatography with fluorescence detection (HPLC-FLD) method was successfully developed for analysing the contamination levels of zearalenone (ZON) and its metabolite α-zearalenol (α-ZOL) in 100 widely consumed foods and medicinal plants in China. Samples were extracted with methanol-water (80:20, v/v), and cleaned up by using an immunoaffinity column. The limits of detection of this developed method for ZON and α-ZOL were 4 µg kg(-1) and 2.5 µg kg(-1) , respectively. Recoveries for the samples spiked with three levels (30, 60 and 300 µg kg(-1) for ZON and α-ZOL) ranged from 85.8% to 96.1% with relative standard deviation (RSD) of 2.6-7.1% for ZON, and from 89.9% to 98.7% with RSD of 1.9-9.2% for α-ZOL. Twelve (12%) of these tested samples were contaminated with ZON at levels ranging from 5.3 to 295.8 µg kg(-1). The most contaminated samples were Semen coicis, four of them in a concentration level exceeding 60 µg kg(-1) 'maximum level' (range 68.9-119.6 µg kg(-1)). Positive samples were further confirmed by liquid chromatography-tandem mass spectrometry. The results suggest that it is necessary to control ZON contamination in medicinal plants, especially Semen coicis. This is a successful study on the analysis of ZON and α-ZOL in medicinal plants in China by HPLC-FLD. Immunoaffinity clean-up and HPLC-FLD proved to have broad applicability in the field of simultaneously detecting ZON and α-ZOL in foods and medicinal plants and other complicated matrices. © 2012 Society of Chemical Industry.

  17. Analytical chromatography. Methods, instrumentation and applications

    International Nuclear Information System (INIS)

    Yashin, Ya I; Yashin, A Ya

    2006-01-01

    The state-of-the-art and the prospects in the development of main methods of analytical chromatography, viz., gas, high performance liquid and ion chromatographic techniques, are characterised. Achievements of the past 10-15 years in the theory and general methodology of chromatography and also in the development of new sorbents, columns and chromatographic instruments are outlined. The use of chromatography in the environmental control, biology, medicine, pharmaceutics, and also for monitoring the quality of foodstuffs and products of chemical, petrochemical and gas industries, etc. is considered.

  18. Potencial de genótipos de trigo duro para produtividade e caracteres agronômicos no Estado de São Paulo Potential of durum wheat genotypes for productivity and agronomic traits in São Paulo State

    Directory of Open Access Journals (Sweden)

    Allan Henrique da Silva

    2010-01-01

    Full Text Available O trigo duro produz a semolina que, extraída dos grãos, é a matéria-prima empregada na elaboração de macarrão. Assim, o objetivo deste estudo foi avaliar o potencial produtivo e comportamento agronômico de 17 linhagens de trigo duro (BH-1146/LGN//2*IAC-1003 oriundas do programa de melhoramento do Instituto Agronômico (IAC e três cultivares-controle: IAC-1001, IAC-1002 e IAC-1003, originárias de introduções do Centro Internacional de Melhoramento de Milho e Trigo (CIMMYT, México. Os experimentos foram instalados em Capão Bonito (sequeiro e em Mococa (irrigado, em 2007 e 2008. Foram avaliados os seguintes caracteres: produtividade (kg ha-1, altura das plantas, comprimento da espiga e comprimento do internódio da raque (cm, número de grãos por espiga e massa de cem grãos (g. A tolerância à toxicidade de alumínio foi realizada empregando soluções nutritivas, no laboratório. As cultivares IAC-1001 e IAC-1003 destacaram-se quanto à produção de grãos nos dois locais. As linhagens 2, 9 e 13 possuem porte semianão mais baixo; as linhagens 4, 15 e a cultivar IAC-1001 exibiram espigas mais compridas; as cultivares IAC-1001 e IAC-1002 sobressaíram-se pelo grande número de grãos por espiga; a 'IAC-1003' pelos grãos mais pesados e as linhagens 1, 4, 15 e 17 revelaram maior comprimento do internódio da raque. Houve tendência dos genótipos de porte semianão mais alto serem mais produtivos, com maior número de grãos por espiga e grãos mais pesados. As linhagens obtidas pelo programa de melhoramento do IAC foram tolerantes à toxicidade de alumínio e as cultivares-controle sensíveis.Semolina extracted from grains of durum wheat is used for manufacturing pastas. Therefore, it is of interest to evaluate the yield potential and agronomic behavior of seventeen durum wheat inbred lines (BH-1146/LGN//2*IAC-1003 originated from Instituto Agronômico (IAC breeding program and three check cultivars IAC-1001, IAC-1002 and IAC-1003

  19. Wheat cultivar tolerance to boron deficiency and toxicity in nutrient solution

    Directory of Open Access Journals (Sweden)

    Furlani Ângela Maria Cangiani

    2003-01-01

    Full Text Available Field symptoms of open spikelets in wheat were observed in specific cultivars and supposedly related to low B soils and differential B requirement among cultivars. This study aimed to evaluate the response of four wheat (Triticum aestivum L. cultivars, IAC 24, IAC 60, IAC 287 and IAC 289, to increasing B concentrations in nutrient solution. The experiment was set up in a randomized complete block design, with four replicates and five B concentrations (0.0, 0.05, 0.2, 0.8 and 2.0 mg L-1, during 1997/1998, in a greenhouse. Plants were grown to maturity and evaluated for plant height, spike number and length, open spikelet number, grains per spike, plant parts dry matter, B, P, K, Ca and Mg leaf concentrations and total nutrient contents. The visual symptoms of B deficiency consisted of open spikelets, distorted spikes without grains. 'IAC 60' and 'IAC 287' had higher B efficiency, with the highest grain yields in lower B concentrations. The 'IAC 287' and 'IAC 24' were more tolerant to the highest B concentrations. 'IAC 24' required more B for grain production as compared to the other cultivars. The critical leaf B concentration for deficiency was 25 mg kg-1 of dry matter tissue for all cultivars, and for toxicity were: 44 to 45 mg kg-1 for 'IAC 60' and 'IAC 289'; 228 and 318 mg kg-1 for 'IAC 24' and 'IAC 287', respectively. Except for the highest B level in the nutrient solution, the leaf P, K, Ca and Mg concentrations and whole plant contents were in an adequate range in the plants and did not vary among cultivars.

  20. Chromatography: Are We Getting It Right?

    Science.gov (United States)

    Maitland, Pamela D.; Maitland, David P.

    2002-01-01

    Explains the basics of chromatography which is used to demonstrate the separation of plant photosynthetic pigments. Reports the results of an evaluative study that explored textbook errors in explaining how chromatography works. (Contains 13 references.) (Author/YDS)

  1. Melhoramento do trigo: XVII. comportamento de linhagens de origem mexicana no estado de São Paulo Wheat breeding: XVII. evaluation of mexican inbred lines for the State of São Paulo, Brazil

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo de Oliveira Camargo

    1988-01-01

    Full Text Available Em ensaios instalados nas Estações Experimentais de Monte Alegre do Sul e Tatuí e no município de Maracaí, de 1984 a 1986, estudaram-se 23 linhagens de trigo introduzidas do Centro Internacional de Melhoramento de Milho e Trigo (CIMMYT, México, juntamente com os cultivares IAC-24 e Anahuac. Analisaram-se os seguintes parâmetros: rendimento de grãos, altura de plantas, ciclo em dias da emergência ao florescimento e da emergência à maturação, porcentagem de plantas acamadas, comprimento da espiga, número de grãos por espiga e por espigueta e de espiguetas por espiga, resistência às ferrugens do colmo e da folha em condições de campo e de casa de vegetação, tolerância à toxicidade de Al3+ empregando-se soluções nutritivas, em laboratório. As linhas mexicanas, nominadas como IAC-215, IAC-216, IAC-217 e IAC-219, destacaram-se quanto à produção de grãos, porém não diferiram do cultivar controle IAC-24. As linhagens Festiguay-Tecolote 363.30.6.1 x Ciguena e [4777² x (Frontana/Kenya 58//Newthatch] Gabo/Pavon-76 mostraram-se resistentes às nove raças do agente causal da ferrugem-do-colmo e às seis raças do agente causal da ferrugem-da-folha. Os resultados evidenciaram que são fontes genéticas de grande valor para o programa de melhoramento do trigo no Instituto Agronômico os genótipos seguintes: IAC-215, IAC-216, Yaco"S", IAC-218, Dougga-Bluejay (T-4, Buckbuck"S" - Bulbul"S", com ciclo precoce; IAC-215, Yaco"S" e Jupateco 73-Bluejay, com porte baixo, Bonanza-Yecora F-70/Florence 35.70, com espigas compridas e maior número de espiguetas e de grãos por espiga; Jupateco 73-Bluejay, com grande fertilidade de espigas; [(IAS-58-IAS-55 x Alondra"S"/IAC-5 Alondra"S" - IAS-58 103A x Alondra"S"] e IAC-215, IAC-216, IAC-219 e IAC-24, com tolerância a 10 mg/litro de Al3+.Twenty three Mexican inbred lines and the cultivars IAC-24 and Anahuac were evaluated in field experiments carried out at Monte Alegre do Sul and Tatu

  2. Stationary phases for superheated water chromatography

    International Nuclear Information System (INIS)

    Saha, Shikha

    2002-01-01

    This project focused on the comparison of conventional liquid chromatography and superheated water chromatography. It examined the differences in efficiency and retention of a range of different stationary phases. Alkyl aryl ketones and eight aromatic compounds were separated on PBD-zirconia, Xterra RP 18, Luna C 18 (2) and Oasis HLB columns using conventional LC and superheated water chromatography system. The retention indices were determined in the different eluents. On changing the organic component of the eluent from methanol to acetonitrile to superheated water considerable improvements were found in the peak shapes and column efficiencies on the PBD-zirconia and Oasis HLB columns. PS-DVB, PBD-zirconia and Xterra RP 18 columns have been used in efficiency studies. It was found that simply elevating the column temperature did not increase the efficiency of a separation in superheated water chromatography. The efficiency depended on flow rate, injection volume and also mobile phase preheating system. Although high efficiencies were not achieved with superheated water on PS-DVB and Xterra RP 18 columns, a higher efficiency was achieved on a PBD-zirconia column with superheated water than with 25-35% ACN at room temperature. The proposed theoretical increases in u opt were measured on three columns using superheated water as the mobile phase. The application of the superheated water chromatographic method to the separation of the pungent constituents of ginger by superheated water chromatography-NMR coupling system was studied. The coupling of superheated water chromatography using deuterium oxide to NMR spectroscopy for the separation of dry ginger extract was successful, although the NMR sensitivity in on-line mode coupling system was low. However, four compounds were identified in the ginger extract by stop-flow mode on superheated water chromatography-UV-NMR detection system. (author)

  3. Atomic Force Microscope Mediated Chromatography

    Science.gov (United States)

    Anderson, Mark S.

    2013-01-01

    The atomic force microscope (AFM) is used to inject a sample, provide shear-driven liquid flow over a functionalized substrate, and detect separated components. This is demonstrated using lipophilic dyes and normal phase chromatography. A significant reduction in both size and separation time scales is achieved with a 25-micron-length column scale, and one-second separation times. The approach has general applications to trace chemical and microfluidic analysis. The AFM is now a common tool for ultra-microscopy and nanotechnology. It has also been demonstrated to provide a number of microfluidic functions necessary for miniaturized chromatography. These include injection of sub-femtoliter samples, fluidic switching, and sheardriven pumping. The AFM probe tip can be used to selectively remove surface layers for subsequent microchemical analysis using infrared and tip-enhanced Raman spectroscopy. With its ability to image individual atoms, the AFM is a remarkably sensitive detector that can be used to detect separated components. These diverse functional components of microfluidic manipulation have been combined in this work to demonstrate AFM mediated chromatography. AFM mediated chromatography uses channel-less, shear-driven pumping. This is demonstrated with a thin, aluminum oxide substrate and a non-polar solvent system to separate a mixture of lipophilic dyes. In conventional chromatographic terms, this is analogous to thin-layer chromatography using normal phase alumina substrate with sheardriven pumping provided by the AFM tip-cantilever mechanism. The AFM detection of separated components is accomplished by exploiting the variation in the localized friction of the separated components. The AFM tip-cantilever provides the mechanism for producing shear-induced flows and rapid pumping. Shear-driven chromatography (SDC) is a relatively new concept that overcomes the speed and miniaturization limitations of conventional liquid chromatography. SDC is based on a

  4. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    Science.gov (United States)

    Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high‐molecular‐weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one‐dimensional liquid chromatography, two‐dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two‐dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two‐dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two‐dimensional liquid chromatography separations. PMID:29027363

  5. Extraction chromatography of actinides

    International Nuclear Information System (INIS)

    Muller, W.

    1978-01-01

    Extraction chromatography of actinides in the oxidation state from 2 to 6 is reviewed. Data on using neutral (tbp), basic (substituted ammonium salts) and acidic [di-(2-ethylhexyl)-phosphoric acid (D2EHPA)] extracting agents ketones, esters, alcohols and β-diketones in this method are given. Using the example of actinide separation using D2EHPA, discussed are factors influencing the efficiency of their chromatography separation (nature and particle size of the carrier materials, extracting agents amount on the carrier, temperature and elution rate)

  6. Purification of lignans from Fructus Arctii using off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography.

    Science.gov (United States)

    Yang, Bichao; Xin, Huaxia; Wang, Feier; Cai, Jianfeng; Liu, Yanfang; Fu, Qing; Jin, Yu; Liang, Xinmiao

    2017-08-01

    As a common traditional Chinese medicine, Fructus Arctii has important clinical medical values. Its main components are lignans, which are difficult to separate and analyze because of the complex composition, similar chemical structures, and close properties. In this study, an off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method, as well as an effective sample pretreatment method based on hydrophilic interaction chromatography material, was developed to enrich the minor lignan fractions and obtain high-purity compounds. In total, 12 high-purity compounds were isolated from Fructus Arctii. Their structures were identified by using high-resolution mass spectrometry and nuclear magnetic resonance spectroscopy, which showed that all were lignans and that most of them were isomers. The results demonstrated the effective off-line two-dimensional supercritical fluid chromatography/reversed-phase liquid chromatography method for the purification of lignans from Fructus Arctii. The separation protocol established here will be beneficial for the separation of complex samples from other kinds of natural products. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Optimizing separations in online comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Pirok, Bob W J; Gargano, Andrea F G; Schoenmakers, Peter J

    2018-01-01

    Online comprehensive two-dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two-dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two-dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass spectrometry (e.g. high-molecular-weight polymers), providing important information on the distribution of the sample components along chemical dimensions (molecular weight, charge, lipophilicity, stereochemistry, etc.). Also, in comparison with conventional one-dimensional liquid chromatography, two-dimensional liquid chromatography provides a greater separation power (peak capacity). Because of the additional selectivity and higher peak capacity, the combination of two-dimensional liquid chromatography with mass spectrometry allows for simpler mixtures of compounds to be introduced in the ion source at any given time, improving quantitative analysis by reducing matrix effects. In this review, we summarize the rationale and principles of two-dimensional liquid chromatography experiments, describe advantages and disadvantages of combining different selectivities and discuss strategies to improve the quality of two-dimensional liquid chromatography separations. © 2017 The Authors. Journal of Separation Science published by WILEY-VCH Verlag GmbH & Co. KGaA.

  8. Hearing preservation in retrosigmoid approach of small vestibular schwannomas: prognostic value of the degree of internal auditory canal filling.

    Science.gov (United States)

    Tringali, Stéphane; Ferber-Viart, Chantal; Fuchsmann, Carine; Buiret, Guillaume; Zaouche, Sandra; Dubreuil, Christian

    2010-12-01

    To assess the contribution of preoperative radiologic appearance of vestibular schwannoma (VS) on the magnetic resonance imaging in constructive interference in steady-state sequences and demonstrate if the degree of the internal auditory canal (IAC) filling is correlated with hearing and facial preservation. A group of 278 patients who underwent VS surgery in a tertiary referral center. Retrosigmoid approach surgery. Patients were classified in 4 groups according to the percentage of IAC filling on the preoperative magnetic resonance imaging as Group IAC 1(IAC empty or filled filled from 25% to 50% with free fundus), Group IAC 3 (IAC filled from 50% to 75% with free fundus), and Group IAC 4 (complete filling of the IAC without fundus obliteration). A good correlation was observed between the IAC classification and the rate of hearing and facial preservation. The global rate of postoperative facial palsy was 10.4%. The global rate of hearing preservation in 213 patients with preoperative hearing class A and B was 40.8%. Regression analysis showed that the degree of lateral extension of the VS in the IAC was a strong predictor of hearing preservation ( p facial outcomes in selected patients with possible hearing preservation. In case of patient with small tumor and IAC empty or filled less than 75% and with free fundus, surgery is the treatment of choice for patients with serviceable hearing and the desire to retain it.

  9. Avaliação da resistência de acessos de tomateiro a tospovírus e a geminivírus Evaluation of tomato accessions for tospovirus and geminivirus resistance

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenção

    2004-06-01

    Full Text Available Treze linhagens avançadas e três cultivares de tomateiro foram avaliadas em condições de campo para resistência a tospovírus e a geminivírus, em Campinas (SP. O germoplasma avaliado compreendeu linhagens do grupo IAC e as cultivares Stevens, Franco e IPA-5. Um mesmo experimento foi instalado em duas épocas. Na primeira, o experimento foi conduzido de 12/2001 a 2/2002, e a única espécie de tospovírus incidente foi Tomato chlorotic spot virus (TCSV. Na segunda época, de 7 a 9/2002, houve infecção por Tomato yellow vein streak virus (TYVSV, sendo a avaliação realizada mediante determinação da porcentagem de plantas infectadas e pela intensidade dos sintomas, medida por escala de notas. Não houve discriminação dos tratamentos com base no primeiro critério, mas o uso de notas permitiu a diferenciação do germoplasma, com destaque para a linhagem IAC-S3-16. Considerando-se ambas as épocas, confirmou-se a suscetibilidade de 'IPA-5' aos dois patógenos e demonstrou-se o comportamento de resistência de 'Franco' a TCSV e a TYVSV. Ainda deve ser destacado o desempenho das linhagens IAC-S3-54, IAC-S3-318, IAC-S4-39 e IAC-SVS-1, com baixas porcentagens de infecção por TCSV, e notas de sintomas de TYVSV próximas à média de 'Franco', caracterizando-se como promissoras para obtenção de cultivares com resistência aos dois vírus.Thirteen lines and three commercial tomato cultivars were screened for tospovirus and geminivirus resistance under field conditions, in Campinas, São Paulo State, Brazil. The germplasm comprised advanced IAC lines plus cultivars Stevens, Franco and IPA-5. The same experiment was carried out in two planting seasons. In the first (December 2001 to February 2002, only Tomato chlorotic spot virus (TCSV occurred in the field. In the second (July to September 2002, Tomato yellow vein streak virus (TYVSV was identified in the experimental area, and the evaluation was carried out through counting of infected

  10. Ion mobility: its role in plasma chromatography

    International Nuclear Information System (INIS)

    Mason, E.A.

    1984-01-01

    This paper is a review of the basic physical theory underlying plasma chromatography. Essentially, plasma chromatography simply measures ion mobility. The new feature of plasma chromatography, as compared to aqueous electrophoresis, is the existence of a highly-developed and accurate body of theory that connects gaseous ion mobility and diffusion to the ion molecule interactions in the drift tube. Attention is restricted to phenomena occurring in the drift tube portion of the apparatus

  11. Avaliação de cultivares de amendoim para resistência a Spodoptera frugiperda

    Directory of Open Access Journals (Sweden)

    Aniele Pianoscki de Campos

    2011-01-01

    Full Text Available Este trabalho teve por objetivo identificar cultivares de amendoim com resistência a Spodoptera frugiperda (J. E. Smith (Lepidoptera: Noctuidae, determinando os graus de resistência por meio da análise univariada e multivariada. Utilizaram-se cultivares de amendoim de hábitos de crescimento ereto (IAC 5, IAC 8112, IAC 22 e IAC Tatu ST e rasteiro (IAC 503, IAC 505, IAC 147, IAC 125, IAC Caiapó e IAC Runner 886, semeadas em campo. Lagartas de primeiro ínstar foram individualizadas em placas de Petri forradas com papel filtro umedecido e mantidas sob condições controladas de temperatura (25 ± 2 °C, umidade (60 ± 10% e fotofase (12 horas. Utilizaram-se cinco repetições de dez lagartas (recém-eclodidas, em delineamento inteiramente casualizado. Diariamente, foram fornecidos folíolos novos, lavados com solução de hipoclorito de sódio a 1%. Avaliaram-se a duração (dias, a massa (mg e a viabilidade (% dos períodos larval e pupal, a razão sexual, longevidade e fecundidade. Os dados foram submetidos à análise de variância (teste F e as médias comparadas pelo teste de Tukey (p<0,05, além da análise de agrupamento e de componentes principais. As cultivares de hábito de crescimento ereto, IAC 22, e rasteiro, IAC Runner 886, foram menos adequadas ao desenvolvimento do inseto, interferindo nas fases larval e pupal de S. frugiperda, demonstrando resistência moderada do tipo antibiose.

  12. Ion Chromatography Applications in Wastewater Analysis

    Directory of Open Access Journals (Sweden)

    Rajmund Michalski

    2018-02-01

    Full Text Available Wastewater analysis is an important area in analytical and environmental chemistry. It can be performed with both the classic wet methods and instrumental techniques. The development of new methods, and modification of the existing ones, constitute a major task for researchers. Ion chromatography plays a predominant role in ion determinations with the instrumental methods. It offers several advantages over the conventional methods, such as simultaneous determinations of alkali and alkaline earth cations and ammonia. Ammonium ions cannot be determined by spectroscopic methods. Ion chromatography has been accepted world-wide as a reference method for analyzing anions and cations in water and wastewater due to the fact that it enables the replacement of several individual wet chemistry methods for common ions with one instrumental technique. The following article describes the principles of ion chromatography, such as stationary phases, eluents, detectors, and sample preparation methods. Moreover, the applications of ion chromatography in wastewater analyses and international standards are presented.

  13. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical

  14. Airtight miniaturized chromatography: a safer method for radiopharmaceutical quality control

    International Nuclear Information System (INIS)

    Coupal, J.J.; Shih, W.J.; Ryo, U.Y.

    1988-01-01

    Miniaturized chromatography is widely used for quality control of radiopharmaceuticals. Recently, published chromatography procedures have illustrated or described chromatography chambers open to the air in use, suggesting that volatile toxic mobile phases are harmless to people in the vicinity. The authors describe the results of their search for an inexpensive closed chromatography chamber that can be used to derive safely the benefits from conventional miniaturized chromatography

  15. Agrometeorological parameters for prediction of the maturation period of Arabica coffee cultivars

    Science.gov (United States)

    Pezzopane, José Ricardo Macedo; Salva, Terezinha de Jesus Garcia; de Lima, Valéria Bittencourt; Fazuoli, Luiz Carlos

    2012-09-01

    The objective of this study was to determine the harvest period of coffee fruits based on the relationship between agrometeorological parameters and sucrose accumulation in the seeds. Over the crop years 2004/2005 and 2006/2007, from 150 days after flowering (DAF) onwards, samples of 50 fruits of cultivars Mundo Novo IAC 376-4, Obatã IAC 1669-20 and Catuaí Vermelho IAC 144 were collected from coffee trees located in Campinas, Brazil. The endosperm of the fruits was freeze-dried, ground and analyzed for sucrose content by high-performance liquid chromatography. A weather station provided data to calculate the accumulated growing degree-day (GDD) units, and the reference (ETo) and actual (ETr) evapotranspiration rates. The results showed that the highest rates of sucrose accumulation occurred at the transition from the cane-green to the cherry phenological stage. Models for the estimation of sucrose content during maturation based on meteorological variables exhibited similar or better performance than the DAF variable, with better results for the variables GDD and ETo. The Mundo Novo cultivar reached the highest sucrose level in the endosperm after 2,790 GDD, while cultivar Catuaí attained its maximum sucrose concentration after the accumulated evapotranspiration rate has reached a value of 870 mm. As for cultivar Obatã, the maximum sucrose concentration was predicted with the same degree of accuracy using any of the parameters investigated. For the Obatã cultivar, the values of the variables calculated for the maximum sucrose concentration to be reached were 249 DAF, 3,090 GDD, 1,020 ETo and 900 ETr.

  16. Isolation and purification of six iridoid glycosides from gardenia jasminoides fruit by medium-pressure liquid chromatography combined with macroporous resin chromatography.

    Science.gov (United States)

    Wang, Yun; Liu, Hui; Shen, Lifeng; Yao, Lan; Ma, Yinlian; Yu, Dingrong; Chen, Jianhong; Li, Puling; Chen, Ying; Zhang, Cun

    2015-12-01

    Gardeniae fructus is one of the most frequently used herbs in traditional Chinese medicine. In the present study, a process for the enrichment of six iridoid glycosides from Gardeniae fructus was developed using medium-pressure liquid chromatography combined with macroporous resin and reversed-phase chromatography. The purities of different fractions from Gardeniae fructus were assessed using quantitative high-performance liquid chromatography. After fractionation using HPD-100 column chromatography, a 30% ethanol fraction was selected based on high-performance liquid chromatography and liquid chromatography with mass spectrometry qualitative analysis to separate and purify. Based on the orientation analysis results, six compounds-deacetyl asperulosidic acid methyl ester, gardenoside, ixoroside, scandoside methyl ester, genipin-1-O-β-d-gentiobioside, and geniposide-were successfully isolated and purified in three to four combined steps from Gardeniae fructus. The purities of these compounds were found by high-performance liquid chromatography analysis to be 97.9, 98.1, 95.5, 96.3, 97.1, and 98.7%, respectively. Moreover, their structures were elucidated by NMR spectroscopy and liquid chromatography with tandem mass spectrometry. The separation process was highly efficient, rapid, and accurate, making it a potential approach for the large-scale production of iridoids in the laboratory and providing several marker compounds for quality control. This procedure may be meaningful for the purification of other natural products used in traditional Chinese medicine. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Optimizing separations in online comprehensive two‐dimensional liquid chromatography

    OpenAIRE

    Pirok, Bob W.J.; Gargano, Andrea F.G.; Schoenmakers, Peter J.

    2017-01-01

    Abstract Online comprehensive two‐dimensional liquid chromatography has become an attractive option for the analysis of complex nonvolatile samples found in various fields (e.g. environmental studies, food, life, and polymer sciences). Two‐dimensional liquid chromatography complements the highly popular hyphenated systems that combine liquid chromatography with mass spectrometry. Two‐dimensional liquid chromatography is also applied to the analysis of samples that are not compatible with mass...

  18. Tolerância de cultivares de trigo a diferentes níveis de alumínio em solução nutritiva e no solo Tolerance op wheat cultivars to different levels of aluminum toxicity

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo de Oliveira Camargo

    1981-01-01

    Full Text Available Foram estudados dez cultivares de trigo em soluções nutritivas contendo cinco diferentes níveis de alumínio tóxico. A tolerância foi medida pela capacidade de as raízes primárias continuarem a crescer em solução sem alumínio, após um período prévio de 48 horas em solução contendo uma concentração conhecida de alumínio. Os cultivares Siete Cerros e Tobari-66 foram sensíveis, respectivamente, a 1 e 3 ppm de alumínio. 'Alondra-S-46', 'Alondra-S-45' e 'IAC-17' foram sensíveis a 6 ppm; 'BH-1146', 'IAC-5', 'IAC-18', 'IAC-13' e 'Londrina' foram tolerantes a 10 ppm, porém 'BH-1146', 'IAC-18' e 'IAC-13' foram mais tolerantes que 'IAC-5' e 'Londrina'. Os cultivares BH-1146, IAC-17, Alondra-S-46, Tobari-66 e Siete Cerros foram cultivados em vasos contendo solo ácido mostrando a presença de alumínio. Metade do número de vasos recebeu uma aplicação de calcário. Os resultados desse experimento mostraram que o cultivar BH-1146 diferiu significativamente em produção de grãos por planta de 'Tobari-66', 'Alondra-S-46', 'IAC-17' e 'Siete Cerros'. Esse resultado confirmou a tolerância ao alumínio do cultivar BH-1146, observada quando se empregou solução nutritiva com a presença desse elemento.Ten wheat cultivars were studied to aluminum toxicity using five different levels of this element. The tolerance was measured taking into account the root growth in a aluminum-free complete nutrient solution after a previous Al treatment. With toxic amounts of Al, the primary roots did not grow at all and remained thickned at the tip as a typical Al injury. The wheat cultivars Siete Cerros and Tobari-66 were sensitive to 1 and 3 ppm of aluminum, respectively. The cultivars Alondra-S-46, Alondra-S-45 and IAC-17 were sensitive to 6 ppm. The cultivars BH-1146, IAC-5, IAC-18, IAC-13 and Londrina showed tolerance to 10 ppm but BH-1146, IAC-18 and IAC-13 were more tolerant than IAC-5 and Londrina. The cultivars BH-1146, IAC-17, Alondra-S-46

  19. Extraction chromatography of fission products

    International Nuclear Information System (INIS)

    Bonnevie-Svendsen, M.; Goon, K.

    1978-01-01

    Various cases of using extraction chromatography during analysis of fission products are reviewed. The use of the extraction chromatography method is considered while analysing reprocessed products of nuclear fuel for quantitative radiochemical analysis and control of fission product and actinoide separation during extraction and their chemical state in production solutions. The method is used to obtain pure fractions of typical burnup monitors (neodymium, molybdenum, cerium, cesium, europium, lanthanides) during determination of nuclear fuel burnup degree. While studying the nature of nuclear reactions the method is used to separate quickly short-life isotopes, to purify β-radiator fractions before measuring their half-life periods, to enrich isotopes forming with low output during fission. Examples of using extraction chromatography are given to separate long half-life or stable fission products from spent solutions, to control environment object contamination

  20. Phytochemical analysis of ethanolic extract of Dichrostachys Cinerea W and Arn leaves by a thin layer chromatography, high performance thin layer chromatography and column chromatography

    OpenAIRE

    M Vijayalakshmi; K Periyanayagam; K Kavitha; K Akilandeshwari

    2013-01-01

    Background: The leaves of Dichrostachys cinerea are used as laxative, diuretic, painkiller. It is also used in the treatment of gonorrhoea, boils, oedema, gout, veneral diseases and nasopharyngeal affections, etc. Materials and Methods: The Phytochemical investigation of ethanolic extract of D. cinerea leaves were performed by standard chemical tests, thin layer chromatography (TLC) by using various solvent systems, and by high performance liquid chromatography (HPTLC). Two compounds were...

  1. Flutuação populacional do bicho-mineiro em cultivares de café arábica resistentes à ferrugem Fluctuation of leaf miner population in resistant arabica coffee cultivars to leaf rust

    Directory of Open Access Journals (Sweden)

    Celso Henrique Costa Conceição

    2005-01-01

    Full Text Available A intensidade de infestação pelo bicho-mineiro, Leucoptera coffeella (Guérin-Méneville (Lepidoptera: Lyonetiidae foi investigada nas cultivares Obatã IAC 1669-20 e Tupi IAC 1669-33, com resistência à ferrugem das folhas do cafeeiro, Hemileia vastatrix Berk. et Br., e Ouro Verde Amarelo IAC 4397, suscetível à doença, em ensaios de campo, localizados em Campinas (SP, Brasil. A incidência de ferrugem e a ocorrência de inimigos naturais da praga, assim como o enfolhamento das plantas, foram também observados nas três cultivares. As curvas de flutuação populacional obtidas para Obatã IAC 1669-20 e Tupi IAC 1669-33 revelaram maior incidência do bicho-mineiro entre abril e novembro. Já na cultivar Ouro Verde Amarelo IAC 4397, observaram-se dois picos de infestação, sendo o primeiro em abril-maio e o segundo em agosto-setembro. No entanto, a elevada percentagem de folhas minadas nas cultivares Tupi IAC 1669-33 e Obatã IAC 1669-20 em relação à Ouro Verde Amarelo IAC 4397 não é evidência de maior suscetibilidade à praga, mas sim devido à maior retenção foliar dessas cultivares, em conseqüência da resistência à ferrugem das folhas observada em ambas. De maneira oposta, na cultivar Ouro Verde Amarelo IAC 4397, os sintomas de ataque do bicho-mineiro ocorreram em menor nível especialmente devido a maior queda de folhas. Com base nas diferenças observadas entre as cultivares, sugere-se a adoção de estratégias distintas de manejo da praga.The intensity of infestation of leaf-miner, Leucoptera coffeella (Guérin-Méneville was investigated in coffee cultivars Obatã IAC 1669-20 and Tupi IAC 1669-33, both resistant to the leaf rust agent, Hemileia vastatrix Berk. et Br., and Ouro Verde Amarelo IAC 4397, susceptible to this coffee disease, at field assays in Campinas, SP, Brazil. The incidence of coffee rust and presence of natural enemies, as well as the plant leafiness, were also observed. In Obatã IAC 1669-20 and Tupi

  2. Purification of flavonoids from licorice using an off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method.

    Science.gov (United States)

    Fan, Yunpeng; Fu, Yanhui; Fu, Qing; Cai, Jianfeng; Xin, Huaxia; Dai, Mei; Jin, Yu

    2016-07-01

    An orthogonal (71.9%) off-line preparative two-dimensional normal-phase liquid chromatography/reversed-phase liquid chromatography method coupled with effective sample pretreatment was developed for separation and purification of flavonoids from licorice. Most of the nonflavonoids were firstly removed using a self-made Click TE-Cys (60 μm) solid-phase extraction. In the first dimension, an industrial grade preparative chromatography was employed to purify the crude flavonoids. Click TE-Cys (10 μm) was selected as the stationary phase that provided an excellent separation with high reproducibility. Ethyl acetate/ethanol was selected as the mobile phase owing to their excellent solubility for flavonoids. Flavonoids co-eluted in the first dimension were selected for further purification using reversed-phase liquid chromatography. Multiple compounds could be isolated from one normal-phase fraction and some compounds with bad resolution in one-dimensional liquid chromatography could be prepared in this two-dimensional system owing to the orthogonal separation. Moreover, this two-dimensional liquid chromatography method was beneficial for the preparation of relatively trace flavonoid compounds, which were enriched in the first dimension and further purified in the second dimension. Totally, 24 flavonoid compounds with high purity were obtained. The results demonstrated that the off-line two-dimensional liquid chromatography method was effective for the preparative separation and purification of flavonoids from licorice. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Analysis of pollutants in air and water using gas chromatography and headspace gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Stenner, H.

    1980-01-01

    The combination 'personal sampling' with headspace gas chromatography to determine traces of formaldehyde, phenol and benzene in air is investigated in this work, with the aim of developing maximum workplace concentration values (MWL values). Further possible applications of gas chromatography in trace analysis in the environmentally protected area. The analysis of chromium in waste waters (Cr III as acetyl acetonate complex) is investigated as further possible application, whereby optimum conditions are obtained. A modified flame ionization detector was used to increase the detection sensitivity.

  4. Nanoparticle Analysis by Online Comprehensive Two-Dimensional Liquid Chromatography combining Hydrodynamic Chromatography and Size-Exclusion Chromatography with Intermediate Sample Transformation

    Science.gov (United States)

    2017-01-01

    Polymeric nanoparticles have become indispensable in modern society with a wide array of applications ranging from waterborne coatings to drug-carrier-delivery systems. While a large range of techniques exist to determine a multitude of properties of these particles, relating physicochemical properties of the particle to the chemical structure of the intrinsic polymers is still challenging. A novel, highly orthogonal separation system based on comprehensive two-dimensional liquid chromatography (LC × LC) has been developed. The system combines hydrodynamic chromatography (HDC) in the first-dimension to separate the particles based on their size, with ultrahigh-performance size-exclusion chromatography (SEC) in the second dimension to separate the constituting polymer molecules according to their hydrodynamic radius for each of 80 to 100 separated fractions. A chip-based mixer is incorporated to transform the sample by dissolving the separated nanoparticles from the first-dimension online in tetrahydrofuran. The polymer bands are then focused using stationary-phase-assisted modulation to enhance sensitivity, and the water from the first-dimension eluent is largely eliminated to allow interaction-free SEC. Using the developed system, the combined two-dimensional distribution of the particle-size and the molecular-size of a mixture of various polystyrene (PS) and polyacrylate (PACR) nanoparticles has been obtained within 60 min. PMID:28745485

  5. Inert carriers for column extraction chromatography

    International Nuclear Information System (INIS)

    Katykhin, G.S.

    1978-01-01

    Inert carriers used in column extraction chromatography are reviewed. Such carriers are devided into two large groups: hydrophilic carriers which possess high surface energy and are well wetted only with strongly polar liquids (kieselguhrs, silica gels, glasses, cellulose, Al 2 O 3 ) and water-repellent carriers which possess low surface energy and are well wetted with various organic solvents (polyethylene, polytetrafluorethylene polytrifluorochlorethylene). Properties of various carriers are presented: structure, chemical and radiation stability, adsorption properties, extracting agent capacity. The effect of structure and sizes of particles on the efficiency of chromatography columns is considered. Ways of immovable phase deposition on the carrier and the latter's regeneration. Peculiarities of column packing for preparative and continuous chromatography are discussed

  6. Gel chromatography of sup(99m)Tc-labelled compounds

    International Nuclear Information System (INIS)

    Vilcek, S.; Machan, V.; Kalincak, M.

    1976-01-01

    The present state of gel chromatography of sup(99m)Tc-labelled compounds is reviewed. Examples are given of gel chromatography for preparing labelled compounds and for quality control analysis and the development of new types of sup(99m)Tc-labelled compounds. The factors which influence the gel chromatography of these compounds are discussed, i.e., the nature of the elution agent, the duration of the contact of the gel and the preparation the gel type, the nature of the labelled compound. The GCS method (gel chromatography scanning) is briefly described. The advantages of gel chromatography as compared with other chromatographic techniques for sup(99m)Tc-labelled compounds are summarized. (author)

  7. XII All-Russian conference on gas chromatography. Program. Summary of reports

    International Nuclear Information System (INIS)

    2002-01-01

    Program and summary of reports of the XII All-Russian conference on gas chromatography are performed. The conference took place in Samara, 10-14 June, 2002. Reports on physicochemical regularities of gas chromatography, application of chromatographic methods in atomic energetics are included in the program of the conference. Part of the reports are deleted to the analytical application of the gas chromatography. Adsorbents for the gas chromatography, complex methods, mathematic methods in chromatography, ecological aspects of the gas chromatography [ru

  8. Avaliação de genótipos de cafeeiros Arabica e Robusta no estado do Acre Evaluation of Arabica and Robusta coffee genotypes in the state of Acre

    Directory of Open Access Journals (Sweden)

    Celso Luis Bergo

    2008-02-01

    Full Text Available Conduziu-se este trabalho, com o objetivo de introduzir e avaliar 40 genótipos de cafeeiros das espécies Coffea arabica e Coffea canephora nas condições edafoclimáticas do Estado do Acre, visando disponibilizar aos cafeicultores acreanos, cultivares com melhor potencial produtivo. Da espécie C. arabica foram avaliados genótipos das cultivares Icatu, Bourbon, Mundo Novo, Catuaí, Obatã e Catimor. Da espécie C. canephora foram avaliadas as cultivares Conilon e Robusta, caracterizadas como Grupo Robusta. Os genótipos utilizados foram provenientes do Instituto Agronômico de Campinas (IAC e da Embrapa Rondônia. O experimento foi conduzido no Campo Experimental da Embrapa Acre, Rio Branco, AC, no período de 1995 a 2004. O delineamento experimental foi em blocos casualizados com cinco repetições. As características avaliadas foram: produtividade, altura, diâmetro da copa e vigor. Da espécie C. arabica, grupo Icatu, destacou-se Icatu-PR-182039-1(IAC H 4782-7-788 com produtividade média de café beneficiado de 34 sc/ ha, Icatu IAC-4041; Icatu IAC-2945; Icatu IAC-2944-MT; Icatu IAC-4040 e Icatu IAC-4046 com produtividade variando de 20 a 26 sacas. Para o grupo Catuaí os melhores genótipos foram Obatã IAC 4275, Obatã IAC 1169 e Catimor IAC 4466 com produtividade média de café beneficiado de 49, 45 e 37 sacas por hectare respectivamente. Na espécie C. canephora foram avaliados 8 genótipos das cultivares Conilon e Robusta e quanto à produtividade não houve diferença estatística, observou-se incremento de 7 sacas/ha para a variedade Conilon IAC 66-3 quando comparado ao Conilon plantado na região. Nesta espécie os genótipos apresentaram sintomas de deficiência hídrica na época seca (julho/agosto.This work aimed to introduce and evaluate 40 coffee genotypes of Coffea arabica e Coffea canephora species in soil and weather conditions of Acre and had as main goal to provide cultivars to coffee producers with better potential of

  9. Peak broadening in paper chromatography and related techniques : III. Peak broadening in thin-layer chromatography on cellulose powder

    NARCIS (Netherlands)

    Ligny, C.L. de; Remijnse, A.G.

    1968-01-01

    The mechanism of peak broadening in thin-layer chromatography on cellulose powder was investigated by comparing the peak widths obtained in chromatography with those caused only by diffusion in the cellulose powder, for a set of amino acids of widely differing RF values and six kinds of cellulose

  10. Screening anti-tumor compounds from Ligusticum wallichii using cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry.

    Science.gov (United States)

    Zhang, Tao; Ding, Yuanyuan; An, Hongli; Feng, Liuxin; Wang, Sicen

    2015-07-14

    Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry was developed. Tyrosine 367 Cysteine-HEK293 cells were used as cell membrane stationary phase. Specificity and reproducibility of the cell membrane chromatography was evaluated using 1-tert-butyl-3-{2-[4-(diethylamino)butylamino]-6-(3,5-dimethoxyphenyl)pyrido[2,3-d]pyrimidin-7-yl}urea, Nimodipine and dexamethasone acetate. Then, anti-tumor components acting on Tyrosine 367 Cysteine-fibroblast growth factor receptor 4 were screened and identified from extracts of Ligusticum wallichii. Components from the extract were retained on the cell membrane chromatographic column. The retained fraction was directly eluted into high-performance liquid chromatography with mass spectrometry system for separation and identification. Finally, Levistolide A was identified as an active component from Ligusticum wallichii extracts. The 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide-formazan colorimetric assay revealed that Levistolide A inhibits proliferation of overexpressing the mutated receptor cells with dose-dependent manner. Phosphorylation of fibroblast growth factor receptor 4 was also decrease under Levistolide A treatment. Flex dock simulation verified that Levistolide A could bind with the tyrosine kinase domain of fibroblast growth factor receptor 4. Therefore, Levistolide A screened by the cell membrane chromatography combined with high-performance liquid chromatography and mass spectrometry can arrest cell growth. In conclusion, the two-dimensional high-performance liquid chromatography method can screen and identify potential anti-tumor ingredients which specifically act on the tyrosine kinase domain of the mutated fibroblast growth factor receptor 4. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  11. Evidence that pp60/sup src/, the product of the Rous sarcoma virus src gene, undergoes autophosphorylation

    International Nuclear Information System (INIS)

    Purchio, A.F.

    1982-01-01

    pp60/sup src/, the product of the Rous sarcoma virus src gene, was purified greater than 100,000-fold by a combination of ion-exchange and immunoaffinity chromatography. Incubation of pp60/sup src/ purified in this fashion with [ 32 P-γ]ATP resulted in a single 32 P-labeled protein when analyzed by sodium dodecyl sulfate-polyacryl-amide gel electrophoresis. Staining of these gels with silver nitrate showed a predominant 60,000-dalton polypeptide which migrated with the protein labeled with 32 P in vitro. Partial digestion of this protein with V8 protease after in vitro iodination indicated that it was pp60/sup src/. These results suggest that pp60/sup src/ is able to autophosphorylate

  12. Purification of recombinant budgerigar fledgling disease virus VP1 capsid protein and its ability for in vitro capsid assembly

    Science.gov (United States)

    Rodgers, R. E.; Chang, D.; Cai, X.; Consigli, R. A.; Spooner, B. S. (Principal Investigator)

    1994-01-01

    A recombinant system for the major capsid VP1 protein of budgerigar fledgling disease virus has been established. The VP1 gene was inserted into a truncated form of the pFlag-1 vector and expressed in Escherichia coli. The budgerigar fledgling disease virus VP1 protein was purified to near homogeneity by immunoaffinity chromatography. Fractions containing highly purified VP1 were pooled and found to constitute 3.3% of the original E. coli-expressed VP1 protein. Electron microscopy revealed that the VP1 protein was isolated as pentameric capsomeres. Electron microscopy also revealed that capsid-like particles were formed in vitro from purified VP1 capsomeres with the addition of Ca2+ ions and the removal of chelating and reducing agents.

  13. Chromium Speciation Analysis by Ion Chromatography Coupled ...

    African Journals Online (AJOL)

    Two methods coupling ion chromatography with inductively coupled plasma - optical emission spectroscopy (ICP-OES) were developed for the simultaneous separation and determination of Cr(III) and Cr(VI) species. In the first method, anion chromatography with sodium bicarbonate/carbonate solution as the eluent was ...

  14. Instrument platforms for nano liquid chromatography.

    Science.gov (United States)

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-11-20

    The history of liquid chromatography started more than a century ago and miniaturization and automation are two leading trends in this field. Nanocolumn liquid chromatography (nano LC) and largely synonymous capillary liquid chromatography (capillary LC) are the most recent results of this process where miniaturization of column dimensions and sorbent particle size play crucial role. Very interesting results achieved in the research of extremely miniaturized LC columns at the end of the last century lacked distinctive raison d'être and only advances in mass spectrometry brought a real breakthrough. Configuration of nano LC-electrospray ionization mass spectrometry (LC-ESI-MS) has become a basic tool in bioanalytical chemistry, especially in proteomics. This review discusses and summarizes past and current trends in the realization of nano liquid chromatography (nano LC) platforms. Special attention is given to the mobile phase delivery under nanoflow rates (isocratic, gradient) and sample injection to the nanocolumn. Available detection techniques applied in nano LC separations are also briefly discussed. We followed up the key themes from the original scientific reports over gradual improvements up to the contemporary commercial solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. Genetic divergence of bean genotypes to infestation of Zabrotes subfasciatus (Bohemann (Coleoptera: Bruchidae

    Directory of Open Access Journals (Sweden)

    Eduardo Neves Costa

    2013-12-01

    Full Text Available The aim of this work was to evaluate the genetics divergence of bean genotypes in relation to the oviposition, feeding and development of Zabrotes subfasciatus, determining the degrees of resistance to the weevil. The genotypes used were: IAC Carioca-Tybatã, IAC Fortaleza, IAPAR 81, IAC Carioca-Eté, IAC Galante, IAC Harmonia, IAC Una, IAC Diplomata, BRS Supremo and RAZ 49. Tests were performed in laboratory under controlled humidity, temperature and photophase conditions. In free choice test, 10 g of bean genotypes seeds were distributed in circular openings placed equidistant from each other in aluminum trays, where 70 couples were released. The attractiveness was evaluated 24 hours and seven days after the experiment started, and then the number of eggs was evaluated. In non choice test, 10 g of seeds were used where seven couples of Z. subfasciatus, 24 hours-old, were released, remaining seven days, and after the adults retreat, the total number eggs, viable and unviable eggs, the number and percentage of emerged adults, weight, longevity and period from egg to adult of males and females, sex ratio, dry mass and dry mass consumed by insect were evaluated. In the genotype IAC Harmonia was observed the lower oviposition; RAZ 49 was the most non preference-type resistant for feeding and/or antibiosis-type resistant; BRS Supremo, IAC Carioca-Eté and IAPAR 81 are no preference for feeding and/or antibiosis-type moderate resistant; IAC Galante is susceptible and the other genotypes are highly susceptible to Z. subfasciatus

  16. Schinus terebinthifolius countercurrent chromatography (Part III): Method transfer from small countercurrent chromatography column to preparative centrifugal partition chromatography ones as a part of method development.

    Science.gov (United States)

    das Neves Costa, Fernanda; Hubert, Jane; Borie, Nicolas; Kotland, Alexis; Hewitson, Peter; Ignatova, Svetlana; Renault, Jean-Hugues

    2017-03-03

    Countercurrent chromatography (CCC) and centrifugal partition chromatography (CPC) are support free liquid-liquid chromatography techniques sharing the same basic principles and features. Method transfer has previously been demonstrated for both techniques but never from one to another. This study aimed to show such a feasibility using fractionation of Schinus terebinthifolius berries dichloromethane extract as a case study. Heptane - ethyl acetate - methanol -water (6:1:6:1, v/v/v/v) was used as solvent system with masticadienonic and 3β-masticadienolic acids as target compounds. The optimized separation methodology previously described in Part I and II, was scaled up from an analytical hydrodynamic CCC column (17.4mL) to preparative hydrostatic CPC instruments (250mL and 303mL) as a part of method development. Flow-rate and sample loading were further optimized on CPC. Mobile phase linear velocity is suggested as a transfer invariant parameter if the CPC column contains sufficient number of partition cells. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Ionic liquid stationary phases for gas chromatography.

    Science.gov (United States)

    Poole, Colin F; Poole, Salwa K

    2011-04-01

    This article provides a summary of the development of ionic liquids as stationary phases for gas chromatography beginning with early work on packed columns that established details of the retention mechanism and established working methods to characterize selectivity differences compared with molecular stationary phases through the modern development of multi-centered cation and cross-linked ionic liquids for high-temperature applications in capillary gas chromatography. Since there are many reviews on ionic liquids dealing with all aspects of their chemical and physical properties, the emphasis in this article is placed on the role of gas chromatography played in the design of ionic liquids of low melting point, high thermal stability, high viscosity, and variable selectivity for separations. Ionic liquids provide unprecedented opportunities for extending the selectivity range and temperature-operating range of columns for gas chromatography, an area of separation science that has otherwise been almost stagnant for over a decade. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. High Performance Liquid Chromatography Experiments to Undergraduate Laboratories

    Science.gov (United States)

    Kissinger, Peter T.; And Others

    1977-01-01

    Reviews the principles of liquid chromatography with electrochemical detection (LCEC), an analytical technique that incorporates the advantages of both liquids chromatography and electrochemistry. Also suggests laboratory experiments using this technique. (MLH)

  19. Isotopic separation by ion chromatography

    International Nuclear Information System (INIS)

    Albert, M.G.; Barre, Y.; Neige, R.

    1994-01-01

    The isotopic exchange reaction and the isotopic separation factor are first recalled; the principles of ion chromatography applied to lithium isotope separation are then reviewed (displacement chromatography) and the process is modelled in the view of dimensioning and optimizing the industrial process; the various dimensioning parameters are the isotopic separation factor, the isotopic exchange kinetics and the material flow rate. Effects of the resin type and structure are presented. Dimensioning is also affected by physico-chemical and hydraulic parameters. Industrial implementation features are also discussed. 1 fig., 1 tab., 5 refs

  20. Desenvolvimento de cultivares de antúrio IAC como plantas de vaso no norte do Paraná Performance of Anthurium's cultivars as an ornamental vessel plant in northern Paraná

    Directory of Open Access Journals (Sweden)

    Lúcia Sadayo Assari Takahashi

    2009-09-01

    Full Text Available O gênero Anthurium Schott. (Araceae compreende mais de 600 espécies. Todas são ornamentais e se destacam pela beleza da folhagem. A espécie Anthurium andraeanum Lind. tem a preferência dos consumidores como planta ornamental devido ao tamanho e colorido de suas espatas. O objetivo do trabalho foi avaliar o desenvolvimento, em vaso, de cinco cultivares de A. andraeanum em Londrina, Norte do Paraná. As cultivares 'Parakanã', 'Terena', 'Apalai', 'Ianomami' e 'Rubi' foram produzidas por meio de micropropagação e selecionadas pelo Instituto Agronômico (IAC. O trabalho foi desenvolvido em estufa tipo arco com 80% de sombreamento obtido por tela de polipropileno de cor preta. Foi plantada uma muda por vaso plástico com volume de quatro litros usando como substrato fibra de coco tipo 80. A avaliação do desempenho comparativo foi iniciada, a partir do transplante das mudas. O comprimento do pecíolo, o número de folhas, a largura e o comprimento das espatas e o comprimento da haste floral foram avaliados mensalmente. Houve aumento na altura e no número de folhas das plantas nos três anos de cultivo. As cultivares 'Parakanã', 'Rubi', 'Terena' e 'Apalai' floresceram e tiveram maior desenvolvimento vegetativo sendo recomendadas para o cultivo em vasos no Norte do Paraná.The genus Anthurium Schott. (Araceae comprehends more than 600 species. All species are ornamental and are distinguished by the beauty of their foliage. The Anthurium andraeanum Lind. has the preference of the public as an ornamental plant because of the color and size of its spathes. The objective of this work was to evaluate of five cultivars of A. andraeanum, as vessel plant, in the northern region of Paraná State. The cultivars 'Parakanã', 'Terena', 'Apalai', 'Ianomami' and 'Rubi' produced by micropropagation by Instituto Agronômico (IAC were analyzed. The study was conducted at greenhouse with 80% of shade given by a black colored polypropylene screen. One seedling

  1. The internal acoustic canal - another review area in paediatric sensorineural hearing loss

    International Nuclear Information System (INIS)

    Chetcuti, Karen; Kumbla, Surekha

    2016-01-01

    Morphological abnormalities of the internal acoustic canal (IAC), albeit rare, are sometimes associated with hearing loss in children. We present an illustration of the spectrum of IAC abnormalities together with a brief review of the embryology and anatomy of the IAC and the techniques used when imaging the petrous temporal bone. This review focuses on morphological abnormalities of the IAC together with their clinical implications and impact on clinical management. (orig.)

  2. The internal acoustic canal - another review area in paediatric sensorineural hearing loss

    Energy Technology Data Exchange (ETDEWEB)

    Chetcuti, Karen [The Royal Children' s Hospital, Department of Medical Imaging, Parkville, VIC (Australia); Kumbla, Surekha [The Royal Children' s Hospital, Department of Medical Imaging, Parkville, VIC (Australia); Monash Health, Clayton, VIC (Australia)

    2016-04-15

    Morphological abnormalities of the internal acoustic canal (IAC), albeit rare, are sometimes associated with hearing loss in children. We present an illustration of the spectrum of IAC abnormalities together with a brief review of the embryology and anatomy of the IAC and the techniques used when imaging the petrous temporal bone. This review focuses on morphological abnormalities of the IAC together with their clinical implications and impact on clinical management. (orig.)

  3. [High-performance liquid-liquid chromatography in beverage analysis].

    Science.gov (United States)

    Bricout, J; Koziet, Y; de Carpentrie, B

    1978-01-01

    Liquid liquid chromatography was performed with columns packed with stationary phases chemically bonded to silica microparticules. These columns show a high efficiency and are used very easily. Flavouring compounds like aromatic aldehydes which have a low volatility were analyzed in brandy using a polar phase alkylnitrile. Sapid substances like amarogentin in Gentiana lutea or glyryrrhizin in Glycyrrhiza glabra were determined by reversed phase chromatography. Finally ionizable substances like synthetic dyes can be analyzed by paired ion chromatography witha non polar stationary phase.

  4. Prostate cell membrane chromatography-liquid chromatography-mass spectrometry for screening of active constituents from Uncaria rhynchophylla.

    Science.gov (United States)

    He, Jianyu; Han, Shengli; Yang, Fangfang; Zhou, Nan; Wang, Sicen

    2013-01-01

    Uncaria rhynchophylla is a traditional Chinese medicinal herb used to treat hypertension and convulsive disorders such as epilepsy. Rat prostate cell membrane chromatography combined with liquid chromatography-mass spectrometry (LC-MS) was used to identify active constituents from U. rhynchophylla extracts. Four compounds (corynoxeine, isorhynchophylline, isocorynoxeine and rhynchophylline) were discovered. Competitive binding assay results indicated that the four compounds were in direct competition at a single common binding site and interacted with α1A adrenergic receptors (α1A-AR) in a manner similar to tamsulosin. Affinity constant values of the four compounds binding with α1A-AR were also measured using rat prostate cell membrane chromatography (CMC). Finally, their pharmacodynamic effects were tested on rat caudal arteries. This CMC combined LC-MS system offers a means of drug discovery by screening natural medicinal herbs for new pharmacologically active molecules targeting specific receptors.

  5. performance liquid chromatography

    African Journals Online (AJOL)

    user

    2010-11-22

    Nov 22, 2010 ... ISSN 1684–5315 © 2010 Academic Journals. Full Length Research Paper. Determination ... Key words: Processed food, high-performance liquid chromatography, acrylamide, health hazard. INTRODUCTION. In the year 2002, the ... potatoes, breakfast cereals etc. It was thus confirmed that acrylamide has ...

  6. Development of a high performance liquid chromatography method ...

    African Journals Online (AJOL)

    Development of a high performance liquid chromatography method for simultaneous ... Purpose: To develop and validate a new low-cost high performance liquid chromatography (HPLC) method for ..... Several papers have reported the use of ...

  7. Laboratory and field based evaluation of chromatography ...

    Science.gov (United States)

    The Monitor for AeRosols and GAses in ambient air (MARGA) is an on-line ion-chromatography-based instrument designed for speciation of the inorganic gas and aerosol ammonium-nitrate-sulfate system. Previous work to characterize the performance of the MARGA has been primarily based on field comparison to other measurement methods to evaluate accuracy. While such studies are useful, the underlying reasons for disagreement among methods are not always clear. This study examines aspects of MARGA accuracy and precision specifically related to automated chromatography analysis. Using laboratory standards, analytical accuracy, precision, and method detection limits derived from the MARGA chromatography software are compared to an alternative software package (Chromeleon, Thermo Scientific Dionex). Field measurements are used to further evaluate instrument performance, including the MARGA’s use of an internal LiBr standard to control accuracy. Using gas/aerosol ratios and aerosol neutralization state as a case study, the impact of chromatography on measurement error is assessed. The new generation of on-line chromatography-based gas and particle measurement systems have many advantages, including simultaneous analysis of multiple pollutants. The Monitor for Aerosols and Gases in Ambient Air (MARGA) is such an instrument that is used in North America, Europe, and Asia for atmospheric process studies as well as routine monitoring. While the instrument has been evaluat

  8. Phytochemical Profile of Erythrina variegata by Using High-Performance Liquid Chromatography and Gas Chromatography-Mass Spectroscopy Analyses

    OpenAIRE

    Suriyavathana Muthukrishnan; Subha Palanisamy; Senthilkumar Subramanian; Sumathi Selvaraj; Kavitha Rani Mari; Ramalingam Kuppulingam

    2016-01-01

    Natural products derived from plant sources have been utilized to treat patients with numerous diseases. The phytochemical constituents present in ethanolic leaf extract of Erythrina variegata (ELEV) were identified by using high-performance liquid chromatography (HPLC) and gas chromatography-mass spectroscopy (GC-MS) analyses. Shade dried leaves were powdered and extracted with ethanol for analyses through HPLC to identify selected flavonoids and through GC-MS to identify other molecules. Th...

  9. Electron-capture process and ion mobility spectra in plasma chromatography

    International Nuclear Information System (INIS)

    Karasek, F.W.; Spangler, G.E.

    1981-01-01

    The basic principles of plasma chromatography are introduced and ion mobility relationships presented. The relationships of plasma chromatography to electron-capture detector mechanisms are discussed, including electron energy considerations and electron-capture reactions. A number of experimental studies by plasma chromatography are described. (C.F.)

  10. Chromatography in Industry

    Science.gov (United States)

    Schoenmakers, Peter

    2009-07-01

    This review focuses on the chromatography research that has been carried out within industry or in close cooperation with industry and that has been reported in the scientific literature between 2006 and mid-2008. Companies in the health care sector, such as pharmaceutical and biotechnology companies, are the largest contributors. Industrial research seems to take place in an open environment in cooperation with academia, peer companies, and institutions. Industry appears ready to embrace new technologies as they emerge, but they focus strongly on making chromatography work robustly, reliably, rapidly, and automatically. “Hyphenated” systems that incorporate on-line sample-preparation techniques and mass-spectrometric detection are the rule rather than the exception. Various multidimensional separation methods are finding numerous applications. Strategies aimed at speeding up the development of new chromatographic methods remain the focus of attention. Also, there is a clear trend toward exploring chromatographic methods for parallel processing along with other strategies for high-throughput analysis.

  11. Separation of Chloroplast Pigments Using Reverse Phase Chromatography.

    Science.gov (United States)

    Reese, R. Neil

    1997-01-01

    Presents a protocol that uses reverse phase chromatography for the separation of chloroplast pigments. Provides a simple and relatively safe procedure for use in teaching laboratories. Discusses pigment extraction, chromatography, results, and advantages of the process. (JRH)

  12. Thin-layer chromatography - liquid chromatography, an ideal supplement demonstrated by the separation of lanthanoids

    International Nuclear Information System (INIS)

    Specker, H.; Hufnagel, A.

    1984-01-01

    All lanthanoids have been separated by thin-layer chromatography (TLC) with short retention times by using a mixture of ether/tetrahydrofurane (THF)/bis-(2-ethylhexyl)-phosphate (HDEHP)/nitric acid. The eluent was empirically tested by synergistic effects. The results have been transferred to high-performance liquid chromatography /HPLC). It was possible to use the same eluent in TLC and HPLC both for the analytical separation of all lanthanoids and for the separation of fission products. The experimental experience gained in HPLC could be applied to the pre-concentration of isotopes in TLC. Both methods excellently supplemented each other in the separation of lanthanoids. (orig.) [de

  13. Advances in chromatography of the rare earth elements (review)

    International Nuclear Information System (INIS)

    Oguma, Koichi; Kuroda, Rokuro; Shimizu, Tsuneo.

    1995-01-01

    A review is presented which covers liquid chromatography, gas chromatography, and related techniques. This article intends to describe the chromatographic methods playing an important role in the separation of the rare earth elements. Special attention is paid to the usefulness of various types of liquid chromatography which enable the complete mutual separation of the rare earth elements. Applications are also discussed. (author) 161 refs

  14. 5-O-caffeoylshikimic acid from Solanum somalense leaves: advantage of centrifugal partition chromatography over conventional column chromatography.

    Science.gov (United States)

    Chideh, Saïda; Pilard, Serge; Attoumbré, Jacques; Saguez, Robert; Hassan-Abdallah, Alshaimaa; Cailleu, Dominique; Wadouachi, Anne; Baltora-Rosset, Sylvie

    2014-09-01

    Solanum somalense leaves, used in Djibouti for their medicinal properties, were extracted by MeOH. Because of the high polyphenol and flavonoid contents of the extract, respectively, determined at 80.80 ± 2.13 mg gallic acid equivalent/g dry weight and 24.4 ± 1.01 mg quercetin equivalent/g dry weight, the isolation and purification of the main polyphenols were carried out by silica gel column chromatography and centrifugal partition chromatography. Column chromatography led to 11 enriched fractions requiring further purification, while centrifugal partition chromatography allowed the easy recovery of the main compound of the extract. In a solvent system composed of CHCl3/MeOH/H2O (9.5:10:5), 21.8 mg of this compound at 97% purity was obtained leading to a yield of 2.63%. Its structure was established as 5-O-caffeoylshikimic acid by mass spectrometry and NMR spectroscopy. This work shows that S. somalense leaves contain very high level of 5-O-caffeoylshikimic acid (0.74% dry weight), making it a potential source of production of this secondary metabolite that is not commonly found in nature but could be partly responsible of the medicinal properties of S. somalense leaves. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. EFICIÊNCIA DE ABSORÇÃO E UTILIZAÇÃO DE POTÁSSIO POR PLANTAS DE SOJA EM SOLUÇÃO NUTRITIVA EFFICIENCY OF POTASSIUM UPTAKE AND UTILIZATION BY SOYBEAN PLANTS

    Directory of Open Access Journals (Sweden)

    LUIS VITOR SILVA DO SACRAMENTO

    1998-01-01

    Full Text Available Em casa de vegetação, desenvolveu-se o experimento em blocos casualizados com esquema fatorial 4 x 2 x 3 e três repetições a fim de estudar a influência da idade sobre as relações de eficiência (EAB, eficiência de absorção; EC, eficiência de conversão, e EUK, eficiência de utilização de potássio e sobre o índice de utilização (IU. Os cultivares de soja IAC 17, IAC 18, IAC 11 e FT 2, crescidos em solução nutritiva com dois níveis de potássio (0,50 e 1,82 mmol.L-1, foram coletadas e separadas em folhas inferiores, medianas e superiores, caule e raiz aos 20, 40 e 60 dias após a transferência para a solução nutritiva. Depois da secagem, as partes foram preparadas para a determinação de K. Verificou-se que plantas deficientes, independentemente do cultivar, retranslocaram K tentando manter seu conteúdo nas folhas medianas, a expensas de demais órgãos. Destacam-se, nesse comportamento, 'IAC 18' e 'IAC 11'. Plantas adequadamente nutridas em K apresentaram maior EAB, ocorrendo o contrário para plantas deficientes. 'IAC 17' e 'IAC 18' apresentaram maior EAB em ambas as condições nutricionais em K e 'FT 2', a maior EUK em condições de deficiência, aos 40 dias (antes do início da floração e, a menor, aos 60 dias. 'IAC 11' teve a maior EUK e 'IAC 18', a menor, aos 60 dias. O IU permitiu atribuir critérios de plasticidade aos cultivares ao se adaptarem à deficiência de K. A maior plasticidade foi observada para 'FT 2' aos 40 dias e, para 'IAC 18', aos 60. Plantas K-deficientes foram mais eficazes na EC, produzindo mais matéria seca por unidade do mineral absorvido.A greenhouse experiment was conducted in a factorial design of randomized complete blocks, with three replications, to study plantage response of soybean cultivars on efficiency: update (EAB; conversion (EC and utilization, as well as utilization index (IU by soybean cultivars. Four soybean cultivars (IAC 17, IAC 18, IAC 11 e FT 2 were grown in

  16. Liquid-adsorption chromatography of metal 8-hydroxyquinolinates

    International Nuclear Information System (INIS)

    Basova, E.M.; Bol'shova, T.A.; Shirshova, T.S.

    1988-01-01

    Using the method of liquid-adsorption chromatography separation of 8-hydroxyquinolinates of Cu, Fe, Ga, In, Al, Ni is realized. Thin-layer chromatography (TLC) is used to define the optimum conditions of separation and highly efficient liquid column chromatography (HELC) - for chelate separation. Applicaton of the same sorbent is a very important condition of transition from TLC to HELC. Solica gel Partisil, mobile phase: benzene - isopropanol mixture, containing 1 x 10 -3 M of 8-hydroxyquinoline, are the optimal conditions for the studied chelates separation. But In and Ga in TLC move together, and in HELC they are partially separated, therefore, for their separation the column selectivity should be improved by selection of mobile phase

  17. Production and characterization of monoclonal antibodies (mAbs) against human serum albumin (HSA) for the development of an immunoaffinity system with oriented anti-HSA mAbs as immobilized ligand.

    Science.gov (United States)

    Rajak, Poonam; Vijayalakshmi, M A; Jayaprakash, N S

    2013-05-05

    Proteins present in human serum are of immense importance in the field of biomarker discovery. But, the presence of high-abundant proteins like albumin makes the analysis more challenging because of masking effect on low-abundant proteins. Therefore, removal of albumin using highly specific monoclonal antibodies (mAbs) can potentiate the discovery of low-abundant proteins. In the present study, mAbs against human serum albumin (HSA) were developed and integrated in to an immunoaffinity based system for specific removal of albumin from the serum. Hybridomas were obtained by fusion of Sp2/0 mouse myeloma cells with spleen cells from the mouse immunized with HSA. Five clones (AHSA1-5) producing mAbs specific to HSA were established and characterized by enzyme linked immunosorbent assay (ELISA) and immunoblotting for specificity, sensitivity and affinity in terms of antigen binding. The mAbs were able to bind to both native albumin as well as its glycated isoform. Reactivity of mAbs with different mammalian sera was tested. The affinity constant of the mAbs ranged from 10(8) to 10(9)M(-1). An approach based on oriented immobilization was followed to immobilize purified anti-HSA mAbs on hydrazine activated agarose gel and the dynamic binding capacity of the column was determined. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Assesing Bemisia tabaci (Genn. biotype B resistance in soybean genotypes: Antixenosis and antibiosis Evaluación de la resistencia de genotipos de soya a Bemisia tabaci (Genn. biotipo B: Antixenosis y antibiosis

    Directory of Open Access Journals (Sweden)

    José Paulo Gonçalves Franco da Silva

    2012-12-01

    Full Text Available Since it was first reported in Brazil in the 1990s, the B biotype of silverleaf whitefly (Bemisia tabaci Genn., Hemiptera: Aleyrodidae has been recognized as an important pest in soybeans (Glycine max L., reducing the productivity of this legume species in some areas of the country. As an alternative to chemical control, the use of resistant genotypes represents an important tool for integrated pest management (IPM. This study evaluated the performance of 10 soybean genotypes prior to whitefly infestation, by testing attractiveness and preference for oviposition in the greenhouse and antibiosis in the laboratory. In a multiple-choice test, 'IAC-17' was the least attractive to insects. In a no-choice test, 'IAC-17' was the least attractive for egg deposition, indicating the occurrence of non-preference for oviposition on this genotype. Trichome density was positively correlated with the oviposition site and may be associated with the resistance of 'IAC-17' to infestation. The genotypes 'IAC-PL1', 'IAC-19', 'Conquista', 'IAC-24' and 'IAC-17' extended the insect's life cycle, indicating the occurrence of a small degree of antibiosis and/or non-preference for feeding.Desde que se registró por primera vez en Brasil en la década de 1990, el biotipo B de la mosca-blanca (Bemisia tabaci Genn., Hemiptera: Aleyrodidae, se reconoce como una importante plaga de la soya (Glycine max L. y es lo que reduce la productividad de estas especies de leguminosas en algunas zonas del pais. Como una alternativa al control químico, el uso de genotipos resistentes representa una herramienta importante para la gestión integrada de plagas (MIP. Este trabajo evaluó el comportamiento de 10 genotipos de soya frente al ataque de la mosca-blanca, por medio de ensayos de atractividad y preferencia para ovipostura en invernaderos y antibiosis en laboratorio. En una prueba de elección multiple, 'IAC-17' fue el menos atractivo para los insectos. En una prueba sin elecci

  19. [Column chromatography purification and analysis of biodiesel by transesterification].

    Science.gov (United States)

    Liu, Yang; Yi, Huai-feng; Chen, Yu; Wu, Yu-long; Yang, Ming-de; Chen, Zeng; Tong, Jun-mao

    2012-02-01

    In the present paper, crude biodiesel prepared with sorbifolia oil as raw material by transesterification was purified by column chromatography, then the composition of biodiesel was analyzed by gas chromatography, FTIR, GC-MS and 1H NMR. Column chromatography can separate the crude biodiesel into two fractions: petroleum ether eluted fraction (A1) and methanol eluted fraction (A2). Petroleum ether eluted fraction was mainly biodiesel fraction, which was produced from sorbifolia oil by transesterification, including methyl linoleate, methyl cis-9-octadecenoate and so on; methanol eluted fraction was mainly glycerol fraction, which came from the side reaction of transesterification. The results show that the purity of refined biodiesel increased from 77.51% to 93.872, and the product recovery rate reached up to 91.04% after the purification by column chromatography. The results obtained by FTIR and 1H NMR further showed that the column chromatography can effectively improve the purity of biodiesel. This paper provides a basis for industrialization of purification of biodiesel.

  20. Ochratoxin A in cocoa and chocolate sampled in Canada.

    Science.gov (United States)

    Turcotte, A-M; Scott, P M

    2011-06-01

    In order to determine the levels of ochratoxin A (OTA) in cocoa and cocoa products available in Canada, a previously published analytical method, with minor modifications to the extraction and immunoaffinity clean-up and inclusion of an evaporation step, was initially used (Method I). To improve the low method recoveries (46-61%), 40% methanol was then included in the aqueous sodium bicarbonate extraction solvent (pH 7.8) (Method II). Clean-up was on an Ochratest™ immunoaffinity column and OTA was determined by liquid chromatography (LC) with fluorescence detection. Recoveries of OTA from spiked cocoa powder (0.5 and 5 ng g(-1)) were 75-84%; while recoveries from chocolate were 93-94%. The optimized method was sensitive (limit of quantification (LOQ) = 0.07-0.08 ng g(-1)), accurate (recovery = 75-94%) and precise (coefficient of variation (CV) cocoa and chocolate. Analysis of 32 samples of cocoa powder (16 alkalized and 16 natural) for OTA showed an incidence of 100%, with concentrations ranging from 0.25 to 7.8 ng g(-1); in six samples the OTA level exceeded 2 ng g(-1), the previously considered European Union limit for cocoa. The frequency of detection of OTA in 28 chocolate samples (21 dark or baking chocolate and seven milk chocolate) was also 100% with concentrations ranging from 0.05 to 1.4 ng g(-1); one sample had a level higher than the previously considered European Union limit for chocolate (1 ng g(-1)).

  1. Interfacial area concentration in gas–liquid bubbly to churn flow regimes in large diameter pipes

    International Nuclear Information System (INIS)

    Shen, Xiuzhong; Hibiki, Takashi

    2015-01-01

    Highlights: • A systematic method to predict interfacial area concentration (IAC) is presented. • A correlation for group 1 bubble void fraction is proposed. • Correlations of IAC and bubble diameter are developed for group 1 bubbles. • Correlations of IAC and bubble diameter are developed for group 2 bubbles. • The newly-developed two-group IAC model compares well with collected databases. - Abstract: This study performed a survey on existing correlations for interfacial area concentration (IAC) prediction and collected an IAC experimental database of two-phase flows taken under various flow conditions in large diameter pipes. Although some of these existing correlations were developed by partly using the IAC databases taken in the low-void-fraction two-phase flows in large diameter pipes, no correlation can satisfactorily predict the IAC in the two-phase flows changing from bubbly, cap bubbly to churn flow in the collected database of large diameter pipes. So this study presented a systematic way to predict the IAC for the bubbly-to-churn flows in large diameter pipes by categorizing bubbles into two groups (group 1: spherical or distorted bubble, group 2: cap bubble). A correlation was developed to predict the group 1 void fraction by using the void fraction for all bubble. The group 1 bubble IAC and bubble diameter were modeled by using the key parameters such as group 1 void fraction and bubble Reynolds number based on the analysis of Hibiki and Ishii (2001, 2002) using one-dimensional bubble number density and interfacial area transport equations. The correlations of IAC and bubble diameter for group 2 cap bubbles were developed by taking into account the characteristics of the representative bubbles among the group 2 bubbles and the comparison between a newly-derived drift velocity correlation for large diameter pipes and the existing drift velocity correlation of Kataoka and Ishii (1987) for large diameter pipes. The predictions from the newly

  2. Caracterização química e perfil de ácidos graxos em cultivares de nogueira-macadâmia Chemical characterization and fatty acids profile in macadamia walnut cultivars

    Directory of Open Access Journals (Sweden)

    Luana Aparecida Castilho Maro

    2012-12-01

    Full Text Available A nogueira-macadâmia produz nozes de alto valor no mercado internacional, devido às características nutricionais de suas amêndoas, consideradas uma excelente fonte energética. O objetivo do trabalho foi realizar a caracterização química e o perfil de ácidos graxos em 22 cultivares de nogueira-macadâmia. As cultivares utilizadas foram: 'Edson', 'HAES 788 (Pahala', 'Beaumont 695', 'Flor Rosa', 'IAC 9-20X', 'HAES 344 (Kau', 'Cannon', 'IAC 9-20', 'C160', 'HAES 849', 'IAC 4-12B', 'HAES 816', 'Doroti', '791 Fuji', 'IAC 4-20 (Keaumi', 'HAES 814', 'HAES 722', 'África', 'IAC Campinas-B', 'HAES 246 (Keauhou', 'HAES 741 (Mauka' e 'HAES 842'. Foram quantificados a umidade, extrato etéreo, proteína, cinza e fibra bruta, além disso, extração de óleo e o perfil de ácidos graxos. A maior quantidade de proteína foi registrada na cultivar 'IAC 9-20X'. Quanto ao teor de fibra bruta, as maiores porcentagens foram observadas nas cultivares 'HAES 741' e 'HAES 842'. As amêndoas de todas as cultivares de nogueira-macadâmia analisadas possuem ácidos palmítico e oleico.The walnuts macadamia have a high value on the international market due to their almonds nutritional characteristics considered to be an excellent source of energy. The aim of this work was to evaluate the chemical composition and fatty acid profile of 22 cultivars of almond walnut macadamia. The cultivars tested were: 'Edson', 'HAES 788 (Pahala', 'Beaumont 695', 'Flor Rosa', 'IAC 9-20X', 'HAES 344 (Kau', 'Cannon', 'IAC 9-20', 'C160', 'HAES 849', 'IAC 4-12B', 'HAES 816', 'Doroti', '791 Fuji', 'IAC 4-20 (Keaumi', 'HAES 814', 'HAES 722', 'África', 'IAC Campinas-B', 'HAES 246 (Keauhou', 'HAES 741 (Mauka' and 'HAES 842'. Moisture, fat, protein, ash and crude fiber were analyzed and also oil extraction and fatty acid profile. The highest amount of protein was recorded in 'IAC 9-20X'. The highest percentages of crude fiber content were observed in cultivars 'HAES 741' and 'HAES 842'. The

  3. Produtividade de cultivares de cafeeiros (Coffea arabica L. submetidas a diferentes épocas de parcelamento da adubação Yield of coffee cultivars (Coffea arabica L. under different split-fertilization times

    Directory of Open Access Journals (Sweden)

    Gabriel Ferreira Bartholo

    2003-08-01

    Full Text Available Os experimentos foram instalados na Fazenda Experimental da Epamig em São Sebastião do Paraíso, com o objetivo de estudar o comportamento das cultivares Mundo Novo-IAC 379/19; Icatu Precoce-IAC 3282; Icatu Amarelo-IAC 2944 e Rubi-MG 1192, em relação a épocas de parcelamento de adubação. As respostas das cultivares foram medidas sobre a produção em função das épocas de parcelamento da adubação, demonstrando que a característica estudada foi influenciada pelas combinações das épocas em que foram submetidas. A cultivar Mundo Novo-IAC 379/19 tolerou intervalos maiores entre as adubações no período de outubro a março, e a cultivar Icatu Amarelo-IAC 2944 respondeu de modo significativo a quatro parcelamentos consecutivos com intervalo de 30-40 dias entre as aplicações. Para a cultivar Icatu Precoce-IAC 3282, existem opções de estabelecimento de épocas adequadas, dependendo do início das chuvas. A cultivar Rubi-MG 1192 não respondeu às épocas de parcelamento da adubação.ABSTRACT - The work was conducted at EPAMIG's Experimental Station in São Sebastião do Paraíso, MG, to study the performance of Mundo Novo-IAC 379/19; Icatu Precoce-IAC 3282; Icatu Amarelo-IAC 2944 and Rubi- MG 1192 coffee cultivars, in relation to time and parceling out of fertilization. Cultivar responses were evaluated by yield measurements, with the results showing that this parameter was affected by time in which fertilization was made. Mundo Novo-IAC 379/19 cultivar tolerated broader intervals between the fertilizations from October to March. Icatu Amarelo-IAC 2944 response was significant to four consecutive parceling, with intervals from 30 to 40 days between applications. Icatu Precoce-IAC 3282 cultivar presented other more appropriate time options depending on the start of rainy season. Rubi-MG 1192 cultivar was not responsive to split-fertilization.

  4. High perfomance liquid chromatography in pharmaceutical analyses.

    Science.gov (United States)

    Nikolin, Branko; Imamović, Belma; Medanhodzić-Vuk, Saira; Sober, Miroslav

    2004-05-01

    In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatography replaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography (HPLC) analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1) Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or serum contains numerous endogenous

  5. Large-scale production and properties of human plasma-derived activated Factor VII concentrate.

    Science.gov (United States)

    Tomokiyo, K; Yano, H; Imamura, M; Nakano, Y; Nakagaki, T; Ogata, Y; Terano, T; Miyamoto, S; Funatsu, A

    2003-01-01

    An activated Factor VII (FVIIa) concentrate, prepared from human plasma on a large scale, has to date not been available for clinical use for haemophiliacs with antibodies against FVIII and FIX. In the present study, we attempted to establish a large-scale manufacturing process to obtain plasma-derived FVIIa concentrate with high recovery and safety, and to characterize its biochemical and biological properties. FVII was purified from human cryoprecipitate-poor plasma, by a combination of anion exchange and immunoaffinity chromatography, using Ca2+-dependent anti-FVII monoclonal antibody. To activate FVII, a FVII preparation that was nanofiltered using a Bemberg Microporous Membrane-15 nm was partially converted to FVIIa by autoactivation on an anion-exchange resin. The residual FVII in the FVII and FVIIa mixture was completely activated by further incubating the mixture in the presence of Ca2+ for 18 h at 10 degrees C, without any additional activators. For preparation of the FVIIa concentrate, after dialysis of FVIIa against 20 mm citrate, pH 6.9, containing 13 mm glycine and 240 mm NaCl, the FVIIa preparation was supplemented with 2.5% human albumin (which was first pasteurized at 60 degrees C for 10 h) and lyophilized in vials. To inactivate viruses contaminating the FVIIa concentrate, the lyophilized product was further heated at 65 degrees C for 96 h in a water bath. Total recovery of FVII from 15 000 l of plasma was approximately 40%, and the FVII preparation was fully converted to FVIIa with trace amounts of degraded products (FVIIabeta and FVIIagamma). The specific activity of the FVIIa was approximately 40 U/ micro g. Furthermore, virus-spiking tests demonstrated that immunoaffinity chromatography, nanofiltration and dry-heating effectively removed and inactivated the spiked viruses in the FVIIa. These results indicated that the FVIIa concentrate had both high specific activity and safety. We established a large-scale manufacturing process of human plasma

  6. Osteoblast cell membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry for screening specific active components from traditional Chinese medicines.

    Science.gov (United States)

    Wang, Nani; Zhang, Qiaoyan; Xin, Hailiang; Shou, Dan; Qin, Luping

    2017-11-01

    A method using osteoblast membrane chromatography coupled with liquid chromatography and time-of-flight mass spectrometry was developed to recognize and identify the specific active components from traditional Chinese medicines. Primary rat osteoblasts were used for the preparation of the stationary phase in the cell chromatography method. Retention components from the cell chromatography were collected and analyzed by liquid chromatography with time-of-flight mass spectrometry. This method was applied in screening active components from extracts of four traditional Chinese medicines. In total, 24 potentially active components with different structures were retained by osteoblast cell chromatography. There were five phenolic glucosides and one triterpenoid saponin from Curculigo orchioides Gaertn, two organic acids and ten flavonoids from Epimedium sagittatum Maxim, one phthalide compound and one organic acid from Angelica sinensis Diels, and two flavonoids and two saponins from Anemarrhena asphodeloides Bunge. Among those, four components (icariin, curculigoside, ferulaic acid, and timosaponin BII) were used for in vitro pharmacodynamics validation. They significantly increased the osteoblast proliferation, alkaline phosphatase activity, levels of bone gla protein and collagen type 1, and promoted mineralized nodule formation. The developed method was an effective screening method for finding active components from complex medicines that act on bone diseases. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. Survey of aflatoxins in watermelon seeds from Iran using immunoaffinity column cleanup and HPLC with fluorescence detection.

    Science.gov (United States)

    Feizy, J; Beheshti, H R; Fakoor Janati, S S; Khoshbakht Fahim, N

    2011-01-01

    This survey was undertaken to determine the levels of aflatoxins in melon seeds. Among 65 samples analyzed by liquid chromatography (LC), the results showed that aflatoxin B1 (AFB1) was the major toxins in melon seeds, detected in 58 samples (89.2% of the total) at an average concentration of 8.5 ng g(-1). The level of AFB1 in 12 samples exceeded the maximum tolerated level for AFB1 in Iranian (5 ng g(-1)) regulations; in other words, 18.5% of samples were unfit for human consumption.

  8. Pseudo-affinity chromatography of rumen microbial cellulase on ...

    African Journals Online (AJOL)

    Pseudo-affinity chromatography of rumen microbial cellulase on Sepharose- Cibacron Blue F3GA. ... African Journal of Biotechnology ... Pseudo affinity adsorption of bioproducts on Sepharose-cibacron blue F3-GA was subjected to rumen microbial enzyme evaluation through batch binding and column chromatography of ...

  9. Purification of a synthetic pterocarpanquinone by countercurrent chromatography

    International Nuclear Information System (INIS)

    Costa, Fernanda das Neves; Silva, Alcides Jose M. da; Domingos, Jorge L. de Oliveira; Costa, Paulo Roberto R.; Leitao, Gilda G.; Daher Netto, Chaquip

    2012-01-01

    Countercurrent chromatography (CCC) was employed as a useful, fast and economic alternative to conventional chromatography techniques for the purification of a synthetic pterocarpanquinone, LQB-118. The separation was performed in a two-step CCC with the solvent system hexanechloroform- methanol-water 2:1.5:5:2 in both steps. Traditional purification of these reaction products by silica gel column chromatography demanded a large amount of solvent and time, besides allowing the irreversible adsorption of the compound in the column. The use of 1 H NMR for the calculation of KD of target compound is proposed as an alternative for HPLC measurements. (author)

  10. Gas chromatography at the Tritium Laboratory Karlsruhe

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.

    2003-08-01

    Among the analytical techniques (mass spectrometry, laser Raman spectroscopy, gas chromatography, use of ionisation chambers) employed at the Tritium Laboratory Karlsruhe (TLK), gas chromatography plays a prominent role. The main reasons for that are the simplicity of the gas chromatographic separation process, the small space required for the equipment, the low investment costs in comparison to other methods, the robustness of the equipment, the simple and straightforward analysis and the fact that all gas species of interest (with the exception of water) can easily be detected by gas chromatographic means. The conventional gas chromatographs GC1 and GC2 used in the Tritium Measurement Techniques (TMT) System of the TLK and the gas chromatograph GC3 of the experiment CAPER are presented in detail, by discussing their flow diagrams, their major components, the chromatograms measured by means of various detectors, shortcomings and possible improvements. One of the main disadvantages of the conventional gas chromatography is the long retention times required for the analysis of hydrogen gas mixtures. To overcome this disadvantage, micro gas chromatography for hydrogen analysis was developed. Reduction of the retention times by one order of magnitude was achieved. (orig.)

  11. High performance liquid chromatography in pharmaceutical analyses

    Directory of Open Access Journals (Sweden)

    Branko Nikolin

    2004-05-01

    Full Text Available In testing the pre-sale procedure the marketing of drugs and their control in the last ten years, high performance liquid chromatographyreplaced numerous spectroscopic methods and gas chromatography in the quantitative and qualitative analysis. In the first period of HPLC application it was thought that it would become a complementary method of gas chromatography, however, today it has nearly completely replaced gas chromatography in pharmaceutical analysis. The application of the liquid mobile phase with the possibility of transformation of mobilized polarity during chromatography and all other modifications of mobile phase depending upon the characteristics of substance which are being tested, is a great advantage in the process of separation in comparison to other methods. The greater choice of stationary phase is the next factor which enables realization of good separation. The separation line is connected to specific and sensitive detector systems, spectrafluorimeter, diode detector, electrochemical detector as other hyphernated systems HPLC-MS and HPLC-NMR, are the basic elements on which is based such wide and effective application of the HPLC method. The purpose high performance liquid chromatography(HPLC analysis of any drugs is to confirm the identity of a drug and provide quantitative results and also to monitor the progress of the therapy of a disease.1 Measuring presented on the Fig. 1. is chromatogram obtained for the plasma of depressed patients 12 h before oral administration of dexamethasone. It may also be used to further our understanding of the normal and disease process in the human body trough biomedical and therapeutically research during investigation before of the drugs registration. The analyses of drugs and metabolites in biological fluids, particularly plasma, serum or urine is one of the most demanding but one of the most common uses of high performance of liquid chromatography. Blood, plasma or

  12. Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

    1995-01-01

    The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

  13. Recent applications of gas chromatography with high-resolution mass spectrometry.

    Science.gov (United States)

    Špánik, Ivan; Machyňáková, Andrea

    2018-01-01

    Gas chromatography coupled to high-resolution mass spectrometry is a powerful analytical method that combines excellent separation power of gas chromatography with improved identification based on an accurate mass measurement. These features designate gas chromatography with high-resolution mass spectrometry as the first choice for identification and structure elucidation of unknown volatile and semi-volatile organic compounds. Gas chromatography with high-resolution mass spectrometry quantitative analyses was previously focused on the determination of dioxins and related compounds using magnetic sector type analyzers, a standing requirement of many international standards. The introduction of a quadrupole high-resolution time-of-flight mass analyzer broadened interest in this method and novel applications were developed, especially for multi-target screening purposes. This review is focused on the development and the most interesting applications of gas chromatography coupled to high-resolution mass spectrometry towards analysis of environmental matrices, biological fluids, and food safety since 2010. The main attention is paid to various approaches and applications of gas chromatography coupled to high-resolution mass spectrometry for non-target screening to identify contaminants and to characterize the chemical composition of environmental, food, and biological samples. The most interesting quantitative applications, where a significant contribution of gas chromatography with high-resolution mass spectrometry over the currently used methods is expected, will be discussed as well. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Radial Chromatography for the Separation of Nitroaniline Isomers

    Science.gov (United States)

    Miller, Robert B.; Case, William S.

    2011-01-01

    Separation techniques are usually presented in the undergraduate organic laboratory to teach students how to purify and isolate compounds. Often the concept of liquid chromatography is introduced by having students create "silica gel columns" to separate components of a reaction mixture. Although useful, column chromatography can be a laborious…

  15. Technological quality and utilization of potato tubers Qualidade tecnológica e utilização de tubérculos de batata

    Directory of Open Access Journals (Sweden)

    José Carlos Feltran

    2004-12-01

    Full Text Available Increasing concerns have been verified with regard to the quality factor of potato tubers and their correct form of use and consumption. The purpose of this research was to determine the technological quality of potato tuber cultivars and identify the best forms of use and consumption. A completely randomized experimental design was adopted with 18 treatments represented by cultivars Agata, Apuã (IAC-5977, Aracy (IAC-2, IAC Aracy Ruiva, Asterix, Bintje, Dali, Clone IAC-6090, Itararé (IAC-5986, Laguna, Remarka, Liseta, Mondial, Novita, Oscar, Picasso, Santana, and Solide, with four replications. Specific gravity showed a positive correlation with starch content, texture, pulp pH, and soluble solids, and was negatively correlated with reducing sugars. The technological characteristics represented by specific gravity, dry matter content, texture, starch content, reducing sugars, pulp pH, titrable acidity, and soluble solids are influenced by genotype or cultivar. Cultivars Oscar, Itararé, IAC Aracy Ruiva, Clone IAC-6090, Aracy, Solide, Asterix, Santana, and Laguna were outstanding with best characteristics for frying, mashing and roasting. Mondial, Picasso, Novita, Dali, and Agata are appropriate for boiling, and more specifically for salads. In turn, potato cultivars Apuã, Remarka, Bintje, and Liseta are suitable for mashing and for roasting.Atualmente tem ocorrido crescente preocupação com o fator qualidade da batata e a forma correta de utilização para o consumo. O objetivo deste trabalho foi determinar a qualidade tecnológica dos tubérculos de cultivares de batata, visando identificar a melhor forma de utilização e consumo. O delineamento experimental foi inteiramente casualizado com 18 tratamentos, representados pelos cultivares Agata, Apuã (IAC-5977, Aracy (IAC-2, IAC Aracy Ruiva, Asterix, Bintje, Dali, Clone IAC-6090, Itararé (IAC-5986, Laguna, Remarka, Liseta, Mondial, Novita, Oscar, Picasso, Santana e Solide, com quatro

  16. Inverse colloidal crystal membranes for hydrophobic interaction membrane chromatography.

    Science.gov (United States)

    Vu, Anh T; Wang, Xinying; Wickramasinghe, S Ranil; Yu, Bing; Yuan, Hua; Cong, Hailin; Luo, Yongli; Tang, Jianguo

    2015-08-01

    Hydrophobic interaction membrane chromatography has gained interest due to its excellent performance in the purification of humanized monoclonal antibodies. The membrane material used in hydrophobic interaction membrane chromatography has typically been commercially available polyvinylidene fluoride. In this contribution, newly developed inverse colloidal crystal membranes that have uniform pores, high porosity and, therefore, high surface area for protein binding are used as hydrophobic interaction membrane chromatography membranes for humanized monoclonal antibody immunoglobulin G purification. The capacity of the inverse colloidal crystal membranes developed here is up to ten times greater than commercially available polyvinylidene fluoride membranes with a similar pore size. This work highlights the importance of developing uniform pore size high porosity membranes in order to maximize the capacity of hydrophobic interaction membrane chromatography. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. An experimental and theoretical study on an injection-assisted air-conditioner using R32 in the refrigeration cycle

    International Nuclear Information System (INIS)

    Qv, Dehu; Dong, Bingbing; Cao, Lin; Ni, Long; Wang, Jijin; Shang, Runxin; Yao, Yang

    2017-01-01

    Highlights: • An advanced injection-assisted air-conditioner (IAC) using R32 was proposed. • In the whole day-night cycle, cooling capacity and energy efficiency ratio of the IAC were enhanced dramatically. • The injection duration of 8 s maximized the IAC cooling potential. • Two-phase injection attained the highest exergetic efficiency approximating 50% or more. • The economic and environmental benefits of the IAC were demonstrated. - Abstract: An air-conditioner (AC) that uses refrigerant R32 assisted with one-phase vapor injection shows high energy efficiency and low discharge temperature in the heat-pump cycle, but the performance is not satisfactory in the refrigeration cycle. In this study, an improved injection cycle consisting of one-phase vapor injection mode and two-phase injection mode is proposed and integrated into an AC using R32, which is now referred to as an advanced injection-assisted air-conditioner (IAC). Through an experimental and theoretical study, an optimal injection duration of 8 s is attained for maximizing the refrigeration potential of the IAC. Furthermore, in an entire day–night cycle, both the cooling capacity and energy efficiency ratio (EER) of the IAC within the two-phase injection cycle are enhanced by 25% and 32%, respectively, compared with those of a noninjection-assisted AC. Moreover, two-phase injection offers the highest exergetic efficiency, approximately 50% or more in the refrigeration cycle, exhibiting remarkable thermodynamic performance of the IAC. In addition, compared to the conventional AC using R410A, the IAC using R32 within a two-phase injection cycle demonstrates reasonable payback performance and substantial reduction in carbon dioxide and sulfur dioxide emissions in the refrigeration cycle.

  18. Composição físico-química do mosto e do vinho branco de cultivares de videiras em resposta a porta-enxertos

    Directory of Open Access Journals (Sweden)

    Marlon Jocimar Rodrigues da Silva

    2015-11-01

    Full Text Available Resumo: O objetivo deste trabalho foi avaliar a influência dos porta-enxertos 'IAC 766 Campinas' e '106-8 Mgt Ripária do Traviú' sobre as características físico-químicas do mosto e do vinho das uvas 'IAC 116-31 Rainha', 'IAC 21-14 Madalena' e 'BRS Lorena'. O mosto das uvas foi avaliado quanto ao pH, sólidos solúveis (SS, acidez total (AT e relação SS/AT. No vinho, realizaram-se as seguintes análises físico-químicas: densidade, teor alcoólico; acidez total, volátil e fixa; pH; extrato seco; açúcares redutores; extrato seco reduzido; álcool em peso/extrato seco reduzido; dióxido de enxofre livre e total; índice de polifenóis totais (I 280, polifenóis totais, flavonoides; e atividade antioxidante. As características do mosto da 'IAC 21-14 Madalena' não foram influenciadas pelos porta-enxertos, no entanto, o porta-enxerto 'IAC 766 Campinas' promoveu maior SS/AT no mosto da 'IAC 116-31 Rainha' e menor SS/AT no da 'BRS Lorena. Os porta-enxertos 'IAC 766 Campinas' e '106-8 Mgt Ripária do Traviú' influenciaram o pH e o teor alcoólico do vinho da 'IAC 116-31 Rainha', o extrato seco do vinho da 'IAC 21-14 Madalena' e a acidez fixa do vinho da 'BRS Lorena'. Não houve influência dos porta-enxertos sobre os compostos fenólicos e a atividade antioxidante dos vinhos.

  19. UHPLC: The Greening Face of Liquid Chromatography

    OpenAIRE

    Cielecka-Piontek, Judyta; Zalewski, Przemys?aw; Jeli?ska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) h...

  20. Selection of imprinted nanoparticles by affinity chromatography.

    Science.gov (United States)

    Guerreiro, António R; Chianella, Iva; Piletska, Elena; Whitcombe, Michael J; Piletsky, Sergey A

    2009-04-15

    Soluble molecularly imprinted nanoparticles were synthesised via iniferter initiated polymerisation and separated by size via gel permeation chromatography. Subsequent fractionation of these particles by affinity chromatography allowed the separation of high affinity fractions from the mixture of nanoparticles. Fractions selected this way possess affinity similar to that of natural antibodies (K(d) 6.6x10(-8)) M and were also able to discriminate between related functional analogues of the template.

  1. NÃO-PREFERÊNCIA PARA ALIMENTAÇÃO DA LAGARTA-DO-CARTUCHO EM MILHO

    Directory of Open Access Journals (Sweden)

    LUÍS CLÁUDIO PATERNO SILVEIRA

    1998-01-01

    Full Text Available O objetivo do trabalho foi avaliar a não-preferência para alimentação de lagartas de 1o e de 5o ínstares, de Spodoptera frugiperda, em quatro genótipos de milho: IAC701 N, 'IAC7777', Mp707 e Zapalote Chico (ZC. Os ensaios foram realizados em arenas, com livre chance de escolha pelas lagartas, por 24 horas. Com lagartas recém-eclodidas, 1o ínstar, observou-se não-preferência ao ZC e Mp707, nos quais se encontraram apenas 20% das lagartas, em comparação com IAC701 N e 'IAC7777', onde se concentraram 80% delas. No teste com lagartas de 5o ínstar, o consumo das seções foliares foi cerca de duas vezes maior em `IAC701 N, se comparado a `ZC' e `Mp707'. Concluiu-se que a antixenose ou não-preferência é um dos mecanismos de resistência encontrados em ZC e Mp707, materiais estrangeiros que confirmam, nas condições de Campinas, suas características de resistência.The effect of corn genotypes upon food preferences of Spodoptera frugiperda larvae was evaluated. The genotypes selected were: IAC701 N, an inbred line of Instituto Agronômico de Campinas (IAC, State of São Paulo, Brazil; 'IAC7777', a single hybrid of IAC in which the above inbred line is one of the parents; Mp707, an inbred line of Mississippi State University considered to be resistant to S. frugiperda; and Zapalote Chico (ZC, a Central American corn race referred as resistant to Helicoverpa zea and S. frugiperda. The tests were run in arenas with free choice among treatments. The test with 1st instar larvae indicated that the insects preferred to feed on the genotypes IAC701 N and IAC7777, and a lower percentage of larvae stablished on the leaves of ZC and Mp707. The test with 5th instar larvae indicated a non-preference of the larvae for the leaves of genotypes Mp707 and ZC while IAC701 N was the most preferred with more leaf area consumed. The non-preference for feeding tests leaded to the conclusion that this type of resistance is present in ZC and Mp707. These

  2. Normal and Reversed-Phase Thin Layer Chromatography of Green Leaf Extracts

    Science.gov (United States)

    Sjursnes, Birte Johanne; Kvittingen, Lise; Schmid, Rudolf

    2015-01-01

    Introductory experiments of chromatography are often conducted by separating colored samples, such as inks, dyes, and plant extracts, using filter paper, chalk, or thin layer chromatography (TLC) plates with various solvent systems. Many simple experiments have been reported. The relationship between normal chromatography and reversed-phase…

  3. Agronomic evaluation of coffee tree “Mundo Novo” cv. in Minas Gerais State

    Directory of Open Access Journals (Sweden)

    Bruno de Souza Monte Raso

    2015-08-01

    Full Text Available Aiming of selecting generations of Arabic coffee plants adapted to different coffee regions of the state of Minas Gerais, experiments were conducted in the cities of Três Pontas, Campos Altos and Capelinha. Thirty three progenies from the “Mundo Novo” cv. were evaluated obtained by the genetic improving program of the coffee plants led by the Instituto Agronomico in Campinas. The experiments were carried out in randomized complete block design with four repetitions and six plants by parcel. The yield analysis were performed conjoint for the three sites and six crops. The adaptability and stability of the individual features were evaluated applying the methodology proposed by Annicchiarico (1992, estimating the Confidence Index (Ii and defining as environment the combination between each biennal and each place, that is, nine environments. The parameters fruit maturation stage, floating grains bean/ fruit and bean size were carried out considering the medium of the last two crops, in Três Pontas. The most promising are the IAC 2931, IAC 379-19, IAC 480, IAC 388-6-16 and IAC 379-19-2 because they showed higher stability in the environments and were among the most productive ones in the average of the nine environments, obtaining higher confidence indexes. The progenies IAC 515-8, IAC 501 12, IAC 464 15 have the best percentages of fruit maturation stage, floating grains bean/fruit and bean size.

  4. Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

    Science.gov (United States)

    Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

    2016-10-01

    A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Diagonal chromatography to study plant protein modifications.

    Science.gov (United States)

    Walton, Alan; Tsiatsiani, Liana; Jacques, Silke; Stes, Elisabeth; Messens, Joris; Van Breusegem, Frank; Goormachtig, Sofie; Gevaert, Kris

    2016-08-01

    An interesting asset of diagonal chromatography, which we have introduced for contemporary proteome research, is its high versatility concerning proteomic applications. Indeed, the peptide modification or sorting step that is required between consecutive peptide separations can easily be altered and thereby allows for the enrichment of specific, though different types of peptides. Here, we focus on the application of diagonal chromatography for the study of modifications of plant proteins. In particular, we show how diagonal chromatography allows for studying proteins processed by proteases, protein ubiquitination, and the oxidation of protein-bound methionines. We discuss the actual sorting steps needed for each of these applications and the obtained results. This article is part of a Special Issue entitled: Plant Proteomics--a bridge between fundamental processes and crop production, edited by Dr. Hans-Peter Mock. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Ion-Exchange Chromatography: Basic Principles and Application.

    Science.gov (United States)

    Cummins, Philip M; Rochfort, Keith D; O'Connor, Brendan F

    2017-01-01

    Ion-Exchange Chromatography (IEC) allows for the separation of ionizable molecules on the basis of differences in charge properties. Its large sample-handling capacity, broad applicability (particularly to proteins and enzymes), moderate cost, powerful resolving ability, and ease of scale-up and automation have led to it becoming one of the most versatile and widely used of all liquid chromatography (LC) techniques. In this chapter, we review the basic principles of IEC, as well as the broader criteria for selecting IEC conditions. By way of further illustration, we outline basic laboratory protocols to partially purify a soluble serine peptidase from bovine whole brain tissue, covering crude tissue extract preparation through to partial purification of the target enzyme using anion-exchange chromatography. Protocols for assaying total protein and enzyme activity in both pre- and post-IEC fractions are also described.

  7. Liquid chromatography detection unit, system, and method

    Science.gov (United States)

    Derenzo, Stephen E.; Moses, William W.

    2015-10-27

    An embodiment of a liquid chromatography detection unit includes a fluid channel and a radiation detector. The radiation detector is operable to image a distribution of a radiolabeled compound as the distribution travels along the fluid channel. An embodiment of a liquid chromatography system includes an injector, a separation column, and a radiation detector. The injector is operable to inject a sample that includes a radiolabeled compound into a solvent stream. The position sensitive radiation detector is operable to image a distribution of the radiolabeled compound as the distribution travels along a fluid channel. An embodiment of a method of liquid chromatography includes injecting a sample that comprises radiolabeled compounds into a solvent. The radiolabeled compounds are then separated. A position sensitive radiation detector is employed to image distributions of the radiolabeled compounds as the radiolabeled compounds travel along a fluid channel.

  8. Electrochemical Detectors in HPLC and Ion Chromatography.

    Science.gov (United States)

    Horvai, George; Pungor, ErnÕ

    1989-01-01

    Back in 1952, the renowned Polish electrochemist Wiktor Kemula introduced chromato-polarography, 1 i.e., polaro-graphic detection for liquid chromatography. This technique continued to develop slowly until the early 1970s (for a review see Reference 2) when modem high-performance liquid chromatography (HPLC) emerged. This new, highly efficient chromatographc method could only be. used with detectors ensuring low dispersion. It was not easy to modify the dropping mercury electrode cells to satisfy this requirement. However, at the same time, electroanalytical chemists, who already had much experience in using carbon-based electrodes for oxidative detection in flow analysis, put forward the idea of oxidative amperometric detection in liquid chromatography. 3,4 In this technique, solid or quasi-solid (paste) electrodes were used and this made possible the construction of miniaturized cells with just a few microliter volume.

  9. Introduction to modern liquid chromatography

    National Research Council Canada - National Science Library

    Snyder, Lloyd R; Kirkland, J. J; Dolan, John W

    2010-01-01

    "High-performance liquid chromatography (HPLC) is today the leading technique for chemical analysis and related applications, with an ability to separate, analyze, and/or purify virtually any sample...

  10. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, Tanja C. W.; Schierbeek, Henk; Houtekamer, Marco; van Engeland, Tom; Derrien, Delphine; Stal, Lucas J.; Boschker, Henricus T. S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ(13)C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  11. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of d13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence, although

  12. Comparison of gas chromatography/isotope ratio mass spectrometry and liquid chromatography/isotope ratio mass spectrometry for carbon stable-isotope analysis of carbohydrates

    NARCIS (Netherlands)

    Moerdijk-Poortvliet, T.C.W.; Schierbeek, H.; Houtekamer, M.; van Engeland, T.; Derrien, D.; Stal, L.J.; Boschker, H.T.S.

    2015-01-01

    Rationale: We compared gas chromatography/isotope ratio mass spectrometry (GC/IRMS) and liquid chromatography/isotope ratio mass spectrometry (LC/IRMS) for the measurement of δ13C values in carbohydrates. Contrary to GC/IRMS, no derivatisation is needed for LC/IRMS analysis of carbohydrates. Hence,

  13. Design of preparative-supercritical fluid chromatography.

    Science.gov (United States)

    Rajendran, Arvind

    2012-08-10

    Preparative supercritical fluid chromatography (prep-SFC) is an important separation process in the chromatographers toolbox. Owing to the unique properties of the mobile phase, which is predominantly CO(2), the behavior of SFC is markedly different from high performance liquid chromatography (HPLC). This review article focuses on the scale-up of preparative chromatography. The basics of SFC, with particular focus on highlighting the key differences between SFC and HPLC, are introduced. Then, a framework for rational design of prep-SFC is proposed. This framework is based on obtaining basic system parameters from analytical scale equipment, i.e., with very small amount of material, and performing design and optimization in silico to evaluate process performance and to identify operating conditions for scale-up. The tools required to obtain the input parameters such as adsorption isotherms are discussed and the development of the design and optimization framework is elaborated. Examples from the literature which use this approach for successful scale-up are provided. Finally the design of multi-column SFC systems is discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Two-Dimensional Liquid Chromatography Analysis of Polystyrene/Polybutadiene Block Copolymers.

    Science.gov (United States)

    Lee, Sanghoon; Choi, Heejae; Chang, Taihyun; Staal, Bastiaan

    2018-05-15

    A detailed characterization of a commercial polystyrene/polybutadiene block copolymer material (Styrolux) was carried out using two-dimensional liquid chromatography (2D-LC). The Styrolux is prepared by statistical linking reaction of two different polystyrene- block-polybutadienyl anion precursors with a multivalent linking agent. Therefore, it is a mixture of a number of branched block copolymers different in molecular weight, composition, and chain architecture. While individual LC analysis, including size exclusion chromatography, interaction chromatography, or liquid chromatography at critical condition, is not good enough to resolve all the polymer species, 2D-LC separations coupling two chromatography methods were able to resolve all polymer species present in the sample; at least 13 block copolymer species and a homopolystyrene blended. Four different 2D-LC analyses combining a different pair of two LC methods provide their characteristic separation results. The separation characteristics of the 2D-LC separations are compared to elucidate the elution characteristics of the block copolymer species.

  15. Column Chromatography To Obtain Organic Cation Sorption Isotherms.

    Science.gov (United States)

    Jolin, William C; Sullivan, James; Vasudevan, Dharni; MacKay, Allison A

    2016-08-02

    Column chromatography was evaluated as a method to obtain organic cation sorption isotherms for environmental solids while using the peak skewness to identify the linear range of the sorption isotherm. Custom packed HPLC columns and standard batch sorption techniques were used to intercompare sorption isotherms and solid-water sorption coefficients (Kd) for four organic cations (benzylamine, 2,4-dichlorobenzylamine, phenyltrimethylammonium, oxytetracycline) with two aluminosilicate clay minerals and one soil. A comparison of Freundlich isotherm parameters revealed isotherm linearity or nonlinearity was not significantly different between column chromatography and traditional batch experiments. Importantly, skewness (a metric of eluting peak symmetry) analysis of eluting peaks can establish isotherm linearity, thereby enabling a less labor intensive means to generate the extensive data sets of linear Kd values required for the development of predictive sorption models. Our findings clearly show that column chromatography can reproduce sorption measures from conventional batch experiments with the benefit of lower labor-intensity, faster analysis times, and allow for consistent sorption measures across laboratories with distinct chromatography instrumentation.

  16. Supercritical fluid chromatography for lipid analysis in foodstuffs.

    Science.gov (United States)

    Donato, Paola; Inferrera, Veronica; Sciarrone, Danilo; Mondello, Luigi

    2017-01-01

    The task of lipid analysis has always challenged separation scientists, and new techniques in chromatography were often developed for the separation of lipids; however, no single technique or methodology is yet capable of affording a comprehensive screening of all lipid species and classes. This review acquaints the role of supercritical fluid chromatography within the field of lipid analysis, from the early developed capillary separations based on pure CO 2 , to the most recent techniques employing packed columns under subcritical conditions, including the niche multidimensional techniques using supercritical fluids in at least one of the separation dimensions. A short history of supercritical fluid chromatography will be introduced first, from its early popularity in the late 1980s, to the sudden fall and oblivion until the last decade, experiencing a regain of interest within the chromatographic community. Afterwards, the subject of lipid nomenclature and classification will be briefly dealt with, before discussing the main applications of supercritical fluid chromatography for food analysis, according to the specific class of lipids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Contribution to high-temperature chromatography and high-temperature-gas-chromatography-mass spectrometry of lipids

    International Nuclear Information System (INIS)

    Aichholz, R.

    1998-04-01

    This thesis describes the use of high temperature gas chromatography for the investigation of unusual triacylglycerols, cyanolipids and bees waxes. The used glass capillary columns were pretreated and coated with tailor made synthesized high temperature stable polysiloxane phases. The selective separation properties of the individual columns were tested with a synthetic lipid mixture. Suitable derivatization procedures for the gaschromatographic analyses of neutral lipids, containing multiple bonds as well as hydroxy-, epoxy-, and carboxyl groups, were developed and optimized. Therefore conjugated olefinic-, conjugated olefinic-acetylenic-, hydroxy-, epoxy-, and conjugated olefinic keto triacylglycerols in miscellaneous plant seed oils as well as hydroxy monoesters, diesters and hydroxy diesters in bees waxes could be analysed directly with high temperature gas chromatography for the first time. In order to elucidate the structures of separated lipid compounds, high temperature gas chromatography was coupled to mass spectrometry and tandem mass spectrometry, respectively. Comparable analytical systems are hitherto not commercial available. Therefore instrumental prerequisites for a comprehensive and detailed analysis of seed oils and bees waxes were established. In GC/MS commonly two ionization methods are used, electron impact ionization and chemical ionization. For the analysis of lipids the first is of limited use only. Due to intensive fragmentation only weak molecular ions are observed. In contrast, the chemical ionization yields in better results. Dominant quasi molecular ions enable an unambiguous determination of the molecular weight. Moreover, characteristic fragment ions provide important indications of certain structural features of the examined compounds. Nevertheless, in some cases the chromatographic resolution was insufficient in order to separate all compounds present in natural lipid mixtures. Owing to the selected detection with mass spectrometry

  18. Loading Effects on Resolution in Thin Layer Chromatography and ...

    Indian Academy of Sciences (India)

    Home; Journals; Resonance – Journal of Science Education; Volume 10; Issue 11. Loading Effects on Resolution in Thin Layer Chromatography and Paper Chromatography. K Girigowda V H Mulimani. Classroom Volume 10 Issue 11 November 2005 pp 79-84 ...

  19. Gas Chromatography-Mass Spectroscopic (GC-MS) Analysis of n ...

    African Journals Online (AJOL)

    tuber-regium (synonym Pleurotus tuber regium) using gas chromatography-mass spectroscopic (GC-. MS) techniques. Methods: The n-hexane extract of the sclerotia ... Soxhlet extraction and analysed using gas chromatography-mass spectroscopic (MS) techniques. ..... Phytochemical composition of Pleurotus tuber regium.

  20. 40 CFR 52.770 - Identification of plan.

    Science.gov (United States)

    2010-07-01

    ... for the Bunge Corporation, Globe Industries, Skyline Corporation, and Dubois County Farm Bureau Co-op...; 326 IAC 8-5-5 Graphic Arts Operations. (4) Effective June 8, 1990: 326 IAC 8-1-2 Compliance Methods... Petroleum Refineries, Monitoring, Reports; 326 IAC 8-5-5 Graphic Arts Operations. (88) On February 15, 1990...

  1. Avaliação do enraizamento, desenvolvimento de raízes e parte aérea de porta-enxertos de videira em condições de campo Evaluation of rooting, development of roots and shoot biomass from rootstock of grapevine, in field conditions

    Directory of Open Access Journals (Sweden)

    Marco Antonio Tecchio

    2007-12-01

    Full Text Available Objetivou-se neste trabalho avaliar o enraizamento, a brotação e o desenvolvimento de raízes de diferentes porta-enxertos de videira em condições de campo. Estacas lenhosas dos porta-enxertos '420 A', 'Golia', '5C', '8B', 'RR101-14', 'SO4', '99R', 'Kober 5BB', 'IAC 766', 'IAC 572', 'IAC 571-6', 'Ripária do Traviú' e 'Rupestris du Lot' foram colocadas em canteiro de terra, sem tratamento prévio. O delineamento foi em blocos ao acaso, com cinco repetições e vinte estacas por parcela, com as estacas dispostas em espaçamento de 12 x 5cm. As estacas foram colocadas para enraizar no início de julho e removidas no final de setembro para as avaliações. A porcentagem de estacas enraizadas variou de 79% para 'Ripária do Traviú' a 99% para o 'RR101-14'. Quanto à brotação, o 'Ripária do Traviú' apresentou 47%, 'IAC 571-6', 'IAC 572', '420 A', 'Rupestris du Lot', 'Kober', 'IAC 766', '8B', '5C', apresentaram de 76 a 89% e 'Golia', 'SO4', '99R' e 'RR 101-14' mais de 90%. 'IAC 572' e 'IAC 571-6' apresentaram o menor número de raízes por estaca, no entanto, foram as que apresentaram raízes mais desenvolvidas, seguidas pelo '5C' e 'Rupestris du Lot'. 'Kober 5BB' e 'Ripária do Traviú' apresentaram as raízes menos desenvolvidas. As demais variedades apresentaram valores intermediários. Concluiu-se que, entre todos os porta-enxertos, o 'Ripária do Traviú' apresentou os menores índices de enraizamento e brotação das estacas, nas condições de campo.The goals of this investigation was to evaluate the rooting, budding and development of roots from different rootstock of grapevine, in field conditions. Ligneous cutting of rootstock '420 A', 'Golia', '5C', '8B', 'RR101-14', 'SO4', '99R', 'Kober 5BB', 'IAC 766', 'IAC 572', 'IAC 571-6', 'Ripária do Traviú' and 'Rupestris du Lot' were planted in soil, without previous preparation. The experimental design was done in randomized blocks, with five repetitions and twenty cutting per plot

  2. Optimisation, simulation, and training in ion chromatography - all for free!

    International Nuclear Information System (INIS)

    Dicinoski, G.W.; Shaw, M.J.; Madden, J.E.; Haddad, P.R.

    2001-01-01

    Since its inception in 1975, ion chromatography (IC) has grown to become a powerful separation tool for the analytical chemist. Today, when scientists refer to the term IC, they mean a collection of chromatographic techniques suitable for the separation of inorganic ions and low molecular weight, water-soluble, organic compounds. The range of chromatographic techniques covered by this designation includes: ion-exchange chromatography; reversed-phase ion-interaction chromatography; and ion-exclusion chromatography. The optimization of the IC separation process is extremely time-consuming. A computer simulation software, Virtual Column 2, that accurately mimic retention behaviour in IC, is presented. It is based on large datasets of experimentally measured retention times; an ideal tool for chromatographers

  3. Csaba Horváth and preparative liquid chromatography.

    Science.gov (United States)

    Guiochon, Georges

    2005-06-24

    Few chromatographers have been interested in furthering preparative liquid chromatography. The pioneers, Tswett, Kuhn and Lederer, A.J.P. Martin, Tiselius, isolated fractions but as an intermediate step in the analysis of their samples. The progress in electronics and sensors, and in their miniaturization has lead to the paradoxical situation that the analysts never see the transient pure fractions that their detector quantitates. Yet, over the last 25 years, preparative liquid chromatography has become an important industrial process for the separation, the extraction, and/or the purification of many pharmaceuticals or pharmaceutical intermediates, including pure enantiomers, purified peptides and proteins, compounds that are manufactured at the relatively large industrial scale of a few kilograms to several hundred tons per year. This development that has strongly affected the modem pharmaceutical industry is mainly due to the pioneering work of Csaba Horváth. His work in preparative HPLC was critical at both the practical and the theoretical levels. He was the first scientist in modem times to pay serious attention to the relationships between the curvature of the equilibrium isotherms, the competitive nature of nonlinear isotherms, and the chromatographic band profiles of complex mixtures. The thermodynamics of multi-component phase equilibria and mass transfer kinetics in chromatography attracted his interest and were the focus of ground-breaking contributions. He investigated displacement chromatography, an old method invented by Tiselius that Csaba was first to implement in HPLC. This choice was explained by the essential characteristic of displacement chromatography, in that it delivers fractions that can be far more concentrated than the feed. Remarkably, once the basics of nonlinear chromatography had been mastered in his group, most of the applications that were studied by his coworkers dealt with peptides of various sizes and with proteins. Thus, all

  4. Analysis of lignans in Magnoliae Flos by turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2016-04-01

    In this study, a method coupling turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry was developed for analyzing the lignans in Magnoliae Flos. By the online pretreatment of turbulent flow chromatography solid-phase extraction, the impurities removal and analytes concentration were automatically processed, and the lignans were separated rapidly and well. Seven lignans of Magnoliae Flos including epieudesmin, magnolin, 1-irioresinol-B-dimethyl ether, epi-magnolin, fargesin aschantin, and demethoxyaschantin were identified by comparing their retention behavior, UV spectra, and mass spectra with those of reference substances or literature data. The developed method was validated, and the good results showed that the method was not only automatic and rapid, but also accurate and reliable. The turbulent flow chromatography with online solid-phase extraction and high-performance liquid chromatography with tandem mass spectrometry method holds a high potential to become an effective method for the quality control of lignans in Magnoliae Flos and a useful tool for the analysis of other complex mixtures. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Study of Separation and Identification of the Active Ingredients in Gardenia jasminoides Ellis Based on a Two-Dimensional Liquid Chromatography by Coupling Reversed Phase Liquid Chromatography and Hydrophilic Interaction Liquid Chromatography.

    Science.gov (United States)

    Zhou, Xuan; Chen, Cen; Ye, Xiaolan; Song, Fenyun; Fan, Guorong; Wu, Fuhai

    2017-01-01

    In this paper, by coupling reversed phase liquid chromatography (RPLC) and hydrophilic interaction liquid chromatography (HILIC), a two-dimensional liquid chromatography system was developed for separation and identification of the active ingredients in Gardenia jasminoides Ellis (GJE). By applying the semi-preparative C18 column as the first dimension and the core-shell column as the second dimension, a total of 896 peaks of GJE were separated. Among the 896 peaks, 16 active ingredients including geniposide, gardenoside, gardoside, etc. were identified by mass spectrometry analysis. The results indicated that the proposed two-dimensional RPLC/HILIC system was an effective method for the analysis of GJE and might hold a high potential to become a useful tool for analysis of other complex mixtures. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Detection methods for mycotoxins in cereal grains and cereal products

    Directory of Open Access Journals (Sweden)

    Pascale Michelangelo N.

    2009-01-01

    Full Text Available Analytical methods for mycotoxins in cereals and cereal-based products require three major steps, including extraction, clean-up (to eliminate interferences from the extract and concentrate the analyte, and detection/determination of the toxin (by using suitable analytical instruments/technologies. Clean-up is essential for the analysis of mycotoxins at trace levels, and involves the use of solid phase extraction and multifunctional (e.g. MycoSep® or immunoaffinity columns. Different chromatographic methods are commonly used for quantitative determination of mycotoxins, including gas-chromatography (GC coupled with electron capture, flame ionization or mass spectrometry (MS detectors (mainly for type-A trichothecenes, and high-performance liquid chromatography (HPLC coupled with ultraviolet, diode array, fluorescence or MS detectors. The choice of method depends on the matrix and the mycotoxin to be analyzed. Liquid chromatography-tandem mass spectrometry (LC-MS/MS is spreading rapidly as a promising technique for simultaneous screening, identification and quantitative determination of a large number of mycotoxins. In addition, commercial immunometric assays, such as enzyme-linked immunosorbent assays (ELISA, are frequently used for screening purposes as well. Recently, a variety of emerging methods have been proposed for the analysis of mycotoxins in cereals based on novel technologies, including immunochromatography (i.e. lateral flow devices, fluorescence polarization immunoassays (FPIA, infrared spectroscopy (FT-NIR, molecularly imprinted polymers (MIPs and optical biosensors.

  7. Spiral Countercurrent Chromatography

    Science.gov (United States)

    Ito, Yoichiro; Knight, Martha; Finn, Thomas M.

    2013-01-01

    For many years, high-speed countercurrent chromatography conducted in open tubing coils has been widely used for the separation of natural and synthetic compounds. In this method, the retention of the stationary phase is solely provided by the Archimedean screw effect by rotating the coiled column in the centrifugal force field. However, the system fails to retain enough of the stationary phase for polar solvent systems such as the aqueous–aqueous polymer phase systems. To address this problem, the geometry of the coiled channel was modified to a spiral configuration so that the system could utilize the radially acting centrifugal force. This successfully improved the retention of the stationary phase. Two different types of spiral columns were fabricated: the spiral disk assembly, made by stacking multiple plastic disks with single or four interwoven spiral channels connected in series, and the spiral tube assembly, made by inserting the tetrafluoroethylene tubing into a spiral frame (spiral tube support). The capabilities of these column assemblies were successfully demonstrated by separations of peptides and proteins with polar two-phase solvent systems whose stationary phases had not been well retained in the earlier multilayer coil separation column for high-speed countercurrent chromatography. PMID:23833207

  8. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from a...

  9. Nontumorous enlargement of the internal auditory canal. A risk factor for sensorineural hearing loss? A high resolution CT-study

    Energy Technology Data Exchange (ETDEWEB)

    Stimmer, H.; Rummeny, E.J. [Technical University Munich, Klinikum rechts der Isar (Germany). Dept. of Radiology; Niedermeyer, H.P. [Technical University Munich, Klinikum rechts der Isar (Germany). ENT-Clinic; Kehl, V. [Technical University Munich, Klinikum rechts der Isar (Germany). Inst. for Medical Statistics and Epidemiology

    2015-06-15

    First aim of the study was to define normal shape and diameter of the internal auditory canal (IAC). In the second part the clinical relevance of IAC-enlargement was analyzed, considering also lesions of the subtle structures at the fundus of the internal auditory canal. 440 high resolution CT-scans of the temporal bone were used for retrospective analysis of the internal auditory canal and its fundus region. The mean value of the IAC diameter in axial and coronal plane was determined. In 20 of 440 patients IAC enlargement was found. In the group with pronounced enlargement (3fold SD) nearly all patients suffered from hearing impairment. In some of them we found structural abnormalities near the IAC fundus in the CSF/perilymph border zone. A new CT-based definition of normal shape and diameter of the internal auditory canal is presented. There is some evidence that a pathologic transmission of CSF-pressure in case of IAC-enlargement and/or abnormal fistulous communications could play an important role in the pathophysiology of hearing loss.

  10. Gas chromatography: mass selective detector

    International Nuclear Information System (INIS)

    Lapinskas, R.

    1988-01-01

    The mechanism of mass spectrometry technique directed for detecting molecular structures is described, with some considerations about its operational features. This mass spectrometer is used as a gas chromatography detector. (author)

  11. Size-exclusion chromatography using core-shell particles.

    Science.gov (United States)

    Pirok, Bob W J; Breuer, Pascal; Hoppe, Serafine J M; Chitty, Mike; Welch, Emmet; Farkas, Tivadar; van der Wal, Sjoerd; Peters, Ron; Schoenmakers, Peter J

    2017-02-24

    Size-exclusion chromatography (SEC) is an indispensable technique for the separation of high-molecular-weight analytes and for determining molar-mass distributions. The potential application of SEC as second-dimension separation in comprehensive two-dimensional liquid chromatography demands very short analysis times. Liquid chromatography benefits from the advent of highly efficient core-shell packing materials, but because of the reduced total pore volume these materials have so far not been explored in SEC. The feasibility of using core-shell particles in SEC has been investigated and contemporary core-shell materials were compared with conventional packing materials for SEC. Columns packed with very small core-shell particles showed excellent resolution in specific molar-mass ranges, depending on the pore size. The analysis times were about an order of magnitude shorter than what could be achieved using conventional SEC columns. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Diamond based adsorbents and their application in chromatography.

    Science.gov (United States)

    Peristyy, Anton A; Fedyanina, Olga N; Paull, Brett; Nesterenko, Pavel N

    2014-08-29

    The idea of using diamond and diamond containing materials in separation sciences has attracted a strong interest in the past decade. The combination of a unique range of properties, such as chemical inertness, mechanical, thermal and hydrolytic stability, excellent thermal conductivity with minimal thermal expansion and intriguing adsorption properties makes diamond a promising material for use in various modes of chromatography. This review summarises the recent research on the preparation of diamond and diamond based stationary phases, their properties and chromatographic performance. Special attention is devoted to the dominant retention mechanisms evident for particular diamond containing phases, and their subsequent applicability to various modes of chromatography, including chromatography carried out under conditions of high temperature and pressure. Copyright © 2014 Elsevier B.V. All rights reserved.

  13. Depleting high-abundant and enriching low-abundant proteins in human serum: An evaluation of sample preparation methods using magnetic nanoparticle, chemical depletion and immunoaffinity techniques.

    Science.gov (United States)

    de Jesus, Jemmyson Romário; da Silva Fernandes, Rafael; de Souza Pessôa, Gustavo; Raimundo, Ivo Milton; Arruda, Marco Aurélio Zezzi

    2017-08-01

    The efficiency of three different depletion methods to remove the most abundant proteins, enriching those human serum proteins with low abundance is checked to make more efficient the search and discovery of biomarkers. These methods utilize magnetic nanoparticles (MNPs), chemical reagents (sequential application of dithiothreitol and acetonitrile, DTT/ACN), and commercial apparatus based on immunoaffinity (ProteoMiner, PM). The comparison between methods shows significant removal of abundant protein, remaining in the supernatant at concentrations of 4.6±0.2, 3.6±0.1, and 3.3±0.2µgµL -1 (n=3) for MNPs, DTT/ACN and PM respectively, from a total protein content of 54µgµL -1 . Using GeLC-MS/MS analysis, MNPs depletion shows good efficiency in removing high molecular weight proteins (>80kDa). Due to the synergic effect between the reagents DTT and ACN, DTT/ACN-based depletion offers good performance in the depletion of thiol-rich proteins, such as albumin and transferrin (DTT action), as well as of high molecular weight proteins (ACN action). Furthermore, PM equalization confirms its efficiency in concentrating low-abundant proteins, decreasing the dynamic range of protein levels in human serum. Direct comparison between the treatments reveals 72 proteins identified when using MNP depletion (43 of them exclusively by this method), but only 20 proteins using DTT/ACN (seven exclusively by this method). Additionally, after PM treatment 30 proteins were identified, seven exclusively by this method. Thus, MNPs and DTT/ACN depletion can be simple, quick, cheap, and robust alternatives for immunochemistry-based protein depletion, providing a potential strategy in the search for disease biomarkers. Copyright © 2017 Elsevier B.V. All rights reserved.

  14. Update on Intra-Arterial Chemotherapy for Retinoblastoma

    Directory of Open Access Journals (Sweden)

    Mario Zanaty

    2014-01-01

    Full Text Available The tools for managing retinoblastoma have been increasing in the past decade. While globe-salvage still relies heavily on intravenous chemotherapy, tumors in advanced stage that failed chemotherapy are now referred for intra-arterial chemotherapy (IAC to avoid enucleation. However, IAC still has many obstacles to overcome. We present an update on the indications, complications, limitations, success, and technical aspects of IAC. Given its safety and high efficacy, it is expected that IAC will replace conventional strategies and will become a first-line option even for tumors that are amenable for other strategies.

  15. Rendimento de grãos de trigo e sua relação com as doenças e variáveis climáticas em Capão Bonito de 1994 a 2001 Wheat grain yield and the relationship with diseases and climatic variations in Capão Bonito, in the period 1994 to 2001

    Directory of Open Access Journals (Sweden)

    João Carlos Felicio

    2004-01-01

    Full Text Available A influência do ambiente no rendimento de grãos de genótipos de trigo e sua relação com as doenças causadas pelos fungos causadores da ferrugem-da-folha e das manchas foliares e suas relações com as variáveis climáticas foram avaliadas no período de 1994-2001, no município de Capão Bonito (SP, latitude 24º02' S, longitude 48º 22' W e altitude 702 m. A interação genótipos x anos foi altamente significativa revelando que diferenças climáticas anuais tiveram influência direta no rendimento de grãos. Em 1998, o rendimento médio de grãos foi o melhor do período e em 1994, o pior. Os genótipos IAPAR 60, IAC 60, IAC 120 e BR 18 apresentaram maior rendimento de grãos na média dos anos considerados. IAPAR 60 mostrou instabilidade no rendimento de grãos no período. Os genótipos Anahuac, IAC 120, IAC 356, IAC 342 e IAC 373 foram imunes às raças prevalentes do fungo causador da ferrugem-da-folha. Como as manchas foliares foram favorecidas pelas condições climáticas, sua ocorrência foi generalizada no período. As precipitações pluviais de maio foram as que melhor se correlacionaram com o desenvolvimento dessa doença.The environmental influence on grain yield and its relationship with leaf rust and leaf spots diseases was evaluated in the period 1994-2001, in Capão Bonito, State of São Paulo, Brazil, 24º02' S, 48º 22' W e altitude, 702 m. The genotype x year interaction was highly significant indicating that annual climatic differences have directly affected the grain yield. The averages of grain yield were the highest in 1998 and the lowest in 1994. The genotypes IAPAR 60, IAC 60, IAC 120 and BR 18 showed high grain yield means. IAPAR 60 did not present grain yield stability. The genotypes Anahuac, IAC 120, IAC 356, IAC 342 and IAC 373 are immune to the prevalent races of the fungus causing leaf rust. As the climatic conditions were favorable to the development leaf spot, its occurrence was generalized. Rainfall

  16. Gas chromatography

    International Nuclear Information System (INIS)

    Cram, S.P.; Risby, T.H.; Field, L.R.; Yu, W.L.

    1980-01-01

    In addition to the published literature for the years 1978 - 79, this review of developments in the field of gas chromatography includes earlier articles of particular significance appearing in foreign journals and the patent literature which was not available at the time of the previous review. The articles cited were selected as presenting the most fundamental developments in theory, methodology, and instrumentation. Some applications are cited if they reflect an advance in the state-of-the-art or have particular relevance to new developments. 1149 references are cited

  17. Use of chelating agents as immovable phase in extraction chromatography

    International Nuclear Information System (INIS)

    Sebesta, F.

    1978-01-01

    Extraction chromatography using chelating agents is reviewed. The theory of element extraction by chelating agents and factors influencing this process (pH, extracting agent concentration in organic phase, masking agent concentration in aqueous phase) are briefly considered. The effect of kinetic factors on the extraction chromatography process is discussed. Ways of preparing columns are emphasized. Examples of using chelating reagents in various extraction chromatography systems are given. β-Diketones, oximes, hydroxamic acids, dithizon, diethyl dithiocarbamic acid are chosen as chelating agents

  18. Variação da composição química em cultivares de batata durante seu desenvolvimento Variation in the chemical composition of potato tubers of three cultivars during the growing season

    Directory of Open Access Journals (Sweden)

    Dayse Soave Spoladore

    1985-01-01

    Full Text Available Estudou-se no presente trabalho a dinâmica de acúmulo de substâncias de reserva e glicoalcalóides totais, durante o desenvolvimento de tubérculos de três cultivares de batata - Aracy (IAC-2, Itaiquara (IAC-3551 e Teberê (IAC-4489 - criados e selecionados pela Seção de Raízes e Tubérculos do Instituto Agronômico, no ano agrícola 1982/83, em plantio "das águas" (novembro-janeiro. Os resultados obtidos são referentes às amostragens realizadas aos 64, 79 e 111 dias após o plantio (DAP, e mostraram que o cultivar Aracy acumulou maior quantidade de matéria seca, proteínas, cinzas, polissacarídeos totais e açúcares solúveis por tubérculo.In the rain season of 1982-1983 (November-January, it was studied the dynamics of accumulation of reserve substances and total glycoalkaloids in growing tubers of the Brazilian potato cultivars Aracy (IAC-2, Itaiquara (IAC-355 1 and Teberê (IAC-4489. Data are related to three sampling dates, 64, 79 and 111 days after planting (DAP. Tubers of Aracy (IAC-2 had the highest dry matter, protein, ash, total polisacharides and soluble e sugar contenta.

  19. Advances in immobilized artificial membrane (IAM) chromatography for novel drug discovery.

    Science.gov (United States)

    Tsopelas, Fotios; Vallianatou, Theodosia; Tsantili-Kakoulidou, Anna

    2016-01-01

    The development of immobilized artificial membrane (IAM) chromatography has unfolded new perspectives for the use of chromatographic techniques in drug discovery, combining simulation of the environment of cell membranes with rapid measurements. The present review describes the characteristics of phosphatidylcholine-based stationary phases and analyses the molecular factors governing IAM retention in comparison to n-octanol-water and liposomes partitioning systems as well as to reversed phase chromatography. Other biomimetic stationary phases are also briefly discussed. The potential of IAM chromatography to model permeability through the main physiological barriers and drug membrane interactions is outlined. Further applications to calculate complex pharmacokinetic properties, related to tissue binding, and to screen drug candidates for phospholipidosis, as well as to estimate cell accumulation/retention are surveyed. The ambivalent nature of IAM chromatography, as a border case between passive diffusion and binding, defines its multiple potential applications. However, despite its successful performance in many permeability and drug-membrane interactions studies, IAM chromatography is still used as a supportive and not a stand-alone technique. Further studies looking at IAM chromatography in different biological processes are still required if this technique is to have a more focused and consistent application in drug discovery.

  20. Carbon nanotube based stationary phases for microchip chromatography

    DEFF Research Database (Denmark)

    Mogensen, Klaus Bo; Kutter, Jörg Peter

    2012-01-01

    already been demonstrated in more classical formats, for improved separation performance in gas and liquid chromatography, and for unique applications in solid phase extraction. Carbon nanotubes are now also entering the field of microfluidics, where there is a large potential to be able to provide......The objective of this article is to provide an overview and critical evaluation of the use of carbon nanotubes and related carbon-based nanomaterials for microchip chromatography. The unique properties of carbon nanotubes, such as a very high surface area and intriguing adsorptive behaviour, have...... integrated, tailor-made nanotube columns by means of catalytic growth of the nanotubes inside the fluidic channels. An evaluation of the different implementations of carbon nanotubes and related carbon-based nanomaterials for microfluidic chromatography devices is given in terms of separation performance...

  1. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. 21 CFR 862.2260 - High pressure liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false High pressure liquid chromatography system for... Clinical Laboratory Instruments § 862.2260 High pressure liquid chromatography system for clinical use. (a) Identification. A high pressure liquid chromatography system for clinical use is a device intended to separate...

  3. Defining glycoprotein cancer biomarkers by MS in conjunction with glycoprotein enrichment.

    Science.gov (United States)

    Song, Ehwang; Mechref, Yehia

    2015-01-01

    Protein glycosylation is an important and common post-translational modification. More than 50% of human proteins are believed to be glycosylated to modulate the functionality of proteins. Aberrant glycosylation has been correlated to several diseases, such as inflammatory skin diseases, diabetes mellitus, cardiovascular disorders, rheumatoid arthritis, Alzheimer's and prion diseases, and cancer. Many approved cancer biomarkers are glycoproteins which are not highly abundant proteins. Therefore, effective qualitative and quantitative assessment of glycoproteins entails enrichment methods. This chapter summarizes glycoprotein enrichment methods, including lectin affinity, immunoaffinity, hydrazide chemistry, hydrophilic interaction liquid chromatography, and click chemistry. The use of these enrichment approaches in assessing the qualitative and quantitative changes of glycoproteins in different types of cancers are presented and discussed. This chapter highlights the importance of glycoprotein enrichment techniques for the identification and characterization of new reliable cancer biomarkers.

  4. Occurrence of deoxynivalenol in wheat flour, instant noodle and biscuits commercialised in Brazil.

    Science.gov (United States)

    Almeida, Adriana Palma de; Lamardo, Leda Conceição Antonia; Shundo, Luzia; Silva, Simone Alves da; Navas, Sandra Aparecida; Alaburda, Janete; Ruvieri, Valter; Sabino, Myrna

    2016-12-01

    A total of 134 samples, consisting of 58 wheat flour, 40 instant noodle and 36 biscuits, were analysed for the presence of deoxynivalenol (DON). The samples were obtained from retail markets of the city of São Paulo during the period 2010-2014. DON was determined by high performance liquid chromatography with ultraviolet detection and immunoaffinity sample clean-up. Method validation followed international guidelines. The LOD and LOQ were 60 and 200 µg kg -1 , respectively, considering the three different types of samples analysed. The lowest recovery found in this study was 91.8% with RSD 4.5% for instant noodles. DON was detected in 91.4%, 97.5% and 97.2% of samples wheat flour, instant noodles and biscuits, respectively, resulting in a total of 94.8% with levels ranging from LOD to 1720.0 µg kg -1 .

  5. Bacterial single-stranded DNA-binding proteins are phosphorylated on tyrosine

    DEFF Research Database (Denmark)

    Mijakovic, Ivan; Petranovic, Dina; Macek, B

    2006-01-01

    for phosphotyrosine-containing proteins in Streptomyces griseus by immunoaffinity chromatography identified bacterial SSBs as a novel target of bacterial tyrosine kinases. Since genes encoding protein-tyrosine kinases (PTKs) have not been recognized in streptomycetes, and SSBs from Streptomyces coelicolor (Sc......SSB) and Bacillus subtilis (BsSSB) share 38.7% identity, we used a B.subtilis protein-tyrosine kinase YwqD to phosphorylate two cognate SSBs (BsSSB and YwpH) in vitro. We demonstrate that in vivo phosphorylation of B.subtilis SSB occurs on tyrosine residue 82, and this reaction is affected antagonistically...... by kinase YwqD and phosphatase YwqE. Phosphorylation of B.subtilis SSB increased binding almost 200-fold to single-stranded DNA in vitro. Tyrosine phosphorylation of B.subtilis, S.coelicolor and Escherichia coli SSBs occured while they were expressed in E.coli, indicating that tyrosine phosphorylation...

  6. Avaliação de produtividade de progênies de cafeeiro em dois sistemas de plantio Yield evaluation of coffee plant (Coffea arabica L. progenies in two tillage systems

    Directory of Open Access Journals (Sweden)

    Gladyston Rodrigues Carvalho

    2006-10-01

    Full Text Available Objetivou-se com o presente trabalho analisar a influência do sistema de plantio (adensado e convencional e a produtividade de cafeeiros (Coffea arabica L., resultantes do cruzamento de Catuaí Vermelho IAC 99 com Mundo Novo IAC 379-19. Foram utilizadas 29 progênies, na 4ª geração por autofecundação do 2º retrocruzamento de Catuaí Vermelho com Mundo Novo desenvolvidas pelo programa de Melhoramento Genético do Cafeeiro em Minas Gerais, coordenado pela EPAMIG. Utilizou-se como testemunha 13 cultivares, Topázio MG-1189 e 1189 SL, Catuaí Vermelho IAC-15, IAC-99 e IAC-144, Catuaí Amarelo MG-17, Rubi MG-1192 e 1192SL, Acaiá Cerrado MG-1474 e 1474 SL, Mundo Novo IAC379-19, IAC-376-4 e 376-4 SL. O experimento foi instalado na Fazenda Experimental da EPAMIG, em São Sebastião do Paraíso, MG em janeiro de 1996 no espaçamento de 3,50 x 1,00 m (sistema convencional e 1,80 x 0,60 m (sistema adensado. O delineamento experimental foi em blocos casualizados, sendo os tratamentos compostos por 42 progênies/cultivares com três repetições e seis plantas por parcela com a análise de variância, em parcelas subdivididas, onde cada biênio (agrupamento de colheita foi considerado como uma subparcela. Avaliou-se a produção de grãos em sacas de 60 kg de café beneficiado/ha. Verificou-se nos resultados que a produtividade inicial no sistema adensado foi maior que no sistema convencional, porém com base no desenvolvimento das plantas essa diferença tendeu a diminuir. Para ambos os sistemas de plantio, pode-se utilizar qualquer uma das cultivares uma vez que as mesmas comportaram-se de forma semelhante. As cultivares utilizadas como testemunha que apresentaram as maiores produtividades foram Topázio MG-1189 e 1189 SL, Rubi MG-1192 e 1192SL, Catuaí Vermelho IAC 15 e IAC 144 e Mundo Novo IAC-376-4 e 376-4SL.The present work was carried out in order to analyze the planting system (high and low plant stand influence on coffee trees (Coffea

  7. Expressão fenotípica de clones de seringueira na região noroeste do estado de São Paulo Phenotypic expression of rubber tree clones in the northwestern region of São Paulo state

    Directory of Open Access Journals (Sweden)

    Paulo de Souza Gonçalves

    2006-01-01

    Full Text Available O desenvolvimento de novos clones de seringueira [Hevea brasiliensis (Willd. ex Adr. de Juss. Muell.-Arg.] com alto potencial de produção aliado a outros caracteres secundários desejáveis é de fundamental importância para uma heveicultura sustentável e competitiva. O objetivo deste trabalho foi avaliar a expressão fenotípica de caracteres superiores em 17 clones de seringueira, tendo em vista a escolha dos mais promissores. Em campo, o experimento obedeceu ao delineamento de blocos ao acaso com três repetições e parcelas lineares de seis plantas. Pelos resultados, verificou-se que o clone IAC 40 foi o mais produtivo, com média de 2.316 kg de borracha seca ha-1 ano-1 no período de seis anos, seguido pelo clone IAC 300 (1.921 kg, enquanto o clone-testemunha, RRIM 600 produziu 1.493 kg. Observou-se na maior parte dos clones, crescimento superior em relação à testemunha. A porcentagem de plantas aptas à sangria variou de 40% (IAC 329 a 100% (IAC 327. Exceto nos clones IAC 56, IAC 331 e IAN 3156 com 7,21 mm, 7,18 mm e 6,40 mm respectivamente, em todos os demais notou-se espessura de casca virgem inferior ao clone RRIM 600 (6,38 mm. Com exceção do IAN 3156, os demais clones tiveram baixa incidência de secamento de painel. O bom desempenho de todos os clones IAC e amazônicos (IAN, Fx e RO permite que sejam recomendados para plantio em pequena escala, ao tempo em que serão avaliados para futura recomendação em grande escala envolvendo diferentes ambientes do Estado de São Paulo.The development of new clones with high production combined to other desirable secondary characters is fundamental for a sustainable and competitive rubber tree cultivation. The objective of this study was to evaluate, during a period of 13 years, the phenotypic expression of superior characters of 17 clones of rubber tree grown in the plateau region of São Paulo State, Brazil. The treatments were arranged in a randomized block design with three

  8. Efeito da mucuna e amendoim em rotação com algodoeiro A study on crop rotation for cotton using velvet bean and peanut

    Directory of Open Access Journals (Sweden)

    Carlos A. M. Ferraz

    1977-01-01

    Full Text Available O efeito da rotação de mucuna (Stizolobium atterrimum Piper & Tracy e amendoim (Arachis hypogaea L. e de duas variedades comerciais de algodoeiro, IAC RM3 e IAC 12-2 (Gossypium hirsutum L. foi estudado nos anos agrícolas de 1967/68 a 1972/73. Foram instalados dois ensaios, um em Presidente Bernardes, com fusariose, em solo podzolizado de Lins e Marília var. Lins naturalmente infectado por Fusarium oxysporumf. vasinfectum e o nematóide causador de galhas Meloidogyne incognita (Kofoid & White Chitwood, e outro em Presidente Venceslau, sem fusariose, em latossolo vermelho-escuro f. arenosa não infectado. A variedade comercial IAC RM3 é resistente e a IAC 12-2 é suscetível à fusariose. Para a análise estatística dos dados adotou-se o esquema de parcelas subdivididas, com seis repetições, tendo sido consideradas como parcelas as variedades de algodoeiro IAC RM3 e IAC 12-2, plantadas em 1968/69, 1970/71, 1971/72 e 1972/73, e como subparcelas as culturas em rotação, mucuna, amendoim e as variedades de algodoeiro IAC RM3 e IAC 12-2, plantadas nos anos-agrícolas de 1967/68 e 1969/70. Em solos com fusariose, em 1968/69, e em solos sem fusariose, no ano agrícola de 1970/71, destacou-se o efeito da rotação com mucuna, seguida da rotação com amendoim. Depois do plantio consecutivo de algodoeiro durante três anos (1970/71 a 1972/73, cessaram praticamente os efeitos da rotação para os dois casos. Houve aumento do teor de potássio após o primeiro ano de rotação, sendo maior para a mucuna.The effect of rotation of velvet bean (Stizolobium atterrimum Piper & Tracy, and peanut (Arachis hypogaea L. with two comercial varieties of cotton IAC RM3 and IAC 12-2 (Gossypium hirsutum L. was studied during 1967/68 to 1972/73. One experiment was conducted in a soil naturally infected by Fusarium oxysporum f. vasinfectum (Atk. Snyder & Hansen and by Meloidogyne incognita (Kofoid & White Chitwood, (President Bernardes, State of São Paulo, in

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

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

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

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

    Science.gov (United States)

    Doshi, Gaurav Mahesh; Une, Hemant Devidas

    2016-01-01

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

  11. Intra-Arterial Chemotherapy as Primary Therapy for Retinoblastoma in Infants Less than 3 Months of Age: A Series of 10 Case-Studies.

    Directory of Open Access Journals (Sweden)

    Miaojuan Chen

    Full Text Available Retinoblastoma is the most common primary malignant intra-ocular tumor in children. Although intra-arterial chemotherapy (IAC by selectively infusing chemotherapy through the ophthalmic artery has become an essential technique in the treatment of advanced intra-ocular retinoblastoma in children, the outcome of IAC as primary therapy for infants less than 3 months of age remains unknown. In this retrospective study, we reviewed the outcome of IAC as primary therapy for retinoblastoma in infants less than 3 months of age.We retrospectively reviewed ten retinoblastoma patients attending our center from January 2009 to September 2015 and beginning primary IAC before the age of 3 months. The patient characteristics, overall outcomes and therapy-related complications were assessed.The mean patient age at the first IAC treatment was 10.4 weeks (range 4.9-12.9 weeks. These eyes were classified according to the International Classification of Retinoblastoma (ICRB as group A (n = 0, B (n = 2, C (n = 0, D (n = 9, or E (n = 2. A total of 28 catheterizations were performed, and the procedure was stopped in one patient because of internal carotid artery spasm. Each eye received a mean of 2.6 cycles of IAC (range 2-4 cycles. After IAC with a mean follow-up of 28.3 months (range 9-65 months, tumor regression was observed in 12 of 13 eyes. One eye was enucleated due to tumor progression. All patients are alive and no patient has developed metastatic disease or other malignancies.Our experience suggests IAC as primary therapy is a feasible and promising treatment for retinoblastoma in infants less than 3 months of age.

  12. Numerical evaluation of the five sensor probe method for measurement of local interfacial area concentration of cap bubbles

    International Nuclear Information System (INIS)

    Euh, D.J.; Yun, B.J.; Song, C.H.; Kwon, T.S.; Chung, M.K.; Lee, U.C.

    2000-01-01

    The interfacial area concentration (IAC) is one of the most important parameters in the two-fluid model for two-phase flow analysis. The IAC can be measured by a local conductivity probe method that uses the difference of conductivity between water and air/steam. The number of sensors in the conductivity probe may be differently chosen by considering the flow regime of two-phase flow. The four sensor conductivity probe method predicts the IAC without any assumptions of the bubble shape. The local IAC can be obtained by measuring the three dimensional velocity vector elements at the measuring point, and the directional cosines of the sensors. The five sensor conductivity probe method proposed in this study is based on the four sensor probe method. With the five sensor probe, the local IAC for a given referred measuring area of the probe can be predicted more exactly. In this paper, the mathematical approach of the five sensor probe method for measuring the IAC is described, and a numerical simulation is carried out for ideal cap bubbles of which the sizes and locations are determined by a random number generator. (author)

  13. MRI enhancement of the facial nerve with Gd-DTPA, 2

    International Nuclear Information System (INIS)

    Yanagida, Masahiro

    1993-01-01

    We performed enhanced MRI using Gd-DTPA in 84 patients with facial palsy. After assessing enhancement of the normal facial nerve, we examined enhancement in patients with Bell's palsy and Ramsay Hunt syndrome. In 95% of patients with Bell's palsy, enhancement was obtained in the distal IAC and labyrinthine portions. In 72%, enhancement was significant from the distal IAC portion through the vertical portion. In some of the patients who underwent enhanced MRI twice, increased signal intensity was observed in distal portions such as the vertical portion. In many cases of Ramsay Hunt syndrome, enhancement was seen extensively in the IAC portion through the vertical portion. In the subjects with internal auditory symptoms such as vertigo and tinnitus, enhancement of the IAC portion was seen not only in the facial nerve but also in the vestibular and the cochlear nerves. These results suggest that the vascular permeability of lesions in Bell's palsy may be increased from the distal IAC portion to the vertical portion. Judging from the present findings with Ramsay Hunt syndrome, symptoms related to the enhanced portions suggest that accompanying internal auditory symptoms occur due to inflammation of the IAC portions of cochlear and vestibular nerves. (author)

  14. MRI enhancement of the facial nerve with Gd-DTPA, 2; Investigation of enhanced nerve portions in patients with facial palsy

    Energy Technology Data Exchange (ETDEWEB)

    Yanagida, Masahiro [Kansai Medical School, Moriguchi, Osaka (Japan)

    1993-08-01

    We performed enhanced MRI using Gd-DTPA in 84 patients with facial palsy. After assessing enhancement of the normal facial nerve, we examined enhancement in patients with Bell's palsy and Ramsay Hunt syndrome. In 95% of patients with Bell's palsy, enhancement was obtained in the distal IAC and labyrinthine portions. In 72%, enhancement was significant from the distal IAC portion through the vertical portion. In some of the patients who underwent enhanced MRI twice, increased signal intensity was observed in distal portions such as the vertical portion. In many cases of Ramsay Hunt syndrome, enhancement was seen extensively in the IAC portion through the vertical portion. In the subjects with internal auditory symptoms such as vertigo and tinnitus, enhancement of the IAC portion was seen not only in the facial nerve but also in the vestibular and the cochlear nerves. These results suggest that the vascular permeability of lesions in Bell's palsy may be increased from the distal IAC portion to the vertical portion. Judging from the present findings with Ramsay Hunt syndrome, symptoms related to the enhanced portions suggest that accompanying internal auditory symptoms occur due to inflammation of the IAC portions of cochlear and vestibular nerves. (author).

  15. Ion chromatography of anions in the primary and secondary circuit

    International Nuclear Information System (INIS)

    Brandt, F.; Trost, R.

    1984-01-01

    Ion chromatography - though based on the same, well-established basic principles as gas chromatography and high pressure fluid chromatography - has made an actual breakthrough only in recent years. The adaptability of the process permits the measurement of samples of different composition or concentration. Some of the experience which has been accumulated in the laboratory at Goesgen nuclear power station during the last two years, is reported. This relates particularly to the composition of the samples, the need to use extremely pure calibration samples, the choice of special laboratory accessories and the like. (orig.) [de

  16. An Interference-Aware Admission Control Design for Wireless Mesh Networks

    Directory of Open Access Journals (Sweden)

    Manikantan Shila Devu

    2010-01-01

    Full Text Available In this paper, we present IAC, an interference aware admission control algorithm for use in wireless mesh networks. The core concept of IAC is to use a low overhead dual threshold based approach to share the bandwidth information with its neighbors in the interfering range. As a result, IAC guarantees that the shared wireless bandwidth is not overutilized and the quality of all existing flows are preserved. Moreover, IAC takes into account the intraflow interference effect to estimate the bandwidth consumption of the flow in a multihop path. We have further proposed two approaches of bandwidth allocation, FCFS and MCU, and demonstrated that proper tuning of thresholds can lead to high performance of both schemes. Simulation results illustrate that IAC effectively limits the overutilization of channel resources which in turn results in high throughput, low delay and low packet loss rate for all admitted flows.

  17. RNase-assisted RNA chromatography

    Science.gov (United States)

    Michlewski, Gracjan; Cáceres, Javier F.

    2010-01-01

    RNA chromatography combined with mass spectrometry represents a widely used experimental approach to identify RNA-binding proteins that recognize specific RNA targets. An important drawback of most of these protocols is the high background due to direct or indirect nonspecific binding of cellular proteins to the beads. In many cases this can hamper the detection of individual proteins due to their low levels and/or comigration with contaminating proteins. Increasing the salt concentration during washing steps can reduce background, but at the cost of using less physiological salt concentrations and the likely loss of important RNA-binding proteins that are less stringently bound to a given RNA, as well as the disassembly of protein or ribonucleoprotein complexes. Here, we describe an improved RNA chromatography method that relies on the use of a cocktail of RNases in the elution step. This results in the release of proteins specifically associated with the RNA ligand and almost complete elimination of background noise, allowing a more sensitive and thorough detection of RNA-binding proteins recognizing a specific RNA transcript. PMID:20571124

  18. Theories to support method development in comprehensive two-dimensional liquid chromatography - A review

    NARCIS (Netherlands)

    Bedani, F.; Schoenmakers, P.J.; Janssen, H.-G.

    2012-01-01

    On-line comprehensive two-dimensional liquid chromatography techniques promise to resolve samples that current one-dimensional liquid chromatography methods cannot adequately deal with. To make full use of the potential of two-dimensional liquid chromatography, optimization is required. Optimization

  19. Desempenho de fungos micorrízicos arbusculares na produção de mudas de maracujazeiro-amarelo, em diferentes substratos Arbuscular mycorrhizal fungi performance to produce mycorrhizal passionflower seedlings under different substrates

    Directory of Open Access Journals (Sweden)

    Adriana Parada Dias da Silveira

    2003-01-01

    Full Text Available O trabalho teve por objetivo selecionar fungos micorrízicos arbusculares (FMAs eficientes na promoção do crescimento de mudas de maracujazeiro-amarelo, em substrato esterilizado, com diferentes níveis de fertilidade, em função da adição ou não de matéria orgânica. Foram realizados três experimentos, em casa de vegetação. No primeiro, empregou-se como substrato uma mistura de 2:1:1 de areia, solo (Latossolo Vermelho Eutroférrico e esterco de curral; no segundo, uma mistura de 1:1 de solo e areia e no terceiro, uma mistura de 9:1 de solo e esterco de curral. Os FMAs empregados foram: Acaulospora sp.(IAC-13, Gigaspora margarita, Glomus sp (IAC-27, Acaulospora morrowae, Acaulospora sp. (IAC-44, Acaulospora scrobiculata, Scutellospora heterogama, Glomus clarum,Glomus sp. (IAC-28, Entrophospora colombiana, Glomus etunicatum e Glomus macrocarpum. No terceiro experimento, empregaram-se G. clarum, Glomus sp. (IAC-28, G. margarita, G. etunicatum e G. macrocarpum (IAC-50, uma mistura dessas espécies e populações de fungos nativos, oriundas de solo de uma cultura de maracujá estabelecida no campo e multiplicadas em Brachiaria decumbens, maracujazeiro e amendoinzeiro. Os efeitos positivos da micorrização foram maiores no substrato sem adição de matéria orgânica (esterco de curral, não superando, entretanto, o efeito da sua adição. G. clarum, G. etunicatum e G. margarita promoveram aumento significativo na produção de matéria seca. No substrato com adição de 25% de matéria orgânica, os fungos Acaulospora sp. (IAC- 44 e A. morrowae foram eficientes na promoção do desenvolvimento das mudas, com desempenho comparável ao Glomus sp. (IAC- 28 no substrato com adição de 10% de esterco de curral. G. clarum mostrou efeito parasítico, diminuindo o crescimento das plantas no substrato com 25% de matéria orgânica.The purpose of this study was to select effective arbuscular mycorrhizal fungi (AMF on the production of yellow

  20. Changes in the ultrastructure of soybean cultivars in response to manganese supply in solution culture Alterações na ultra-estrutura de genótipos de soja em resposta ao fornecimento de manganês em solução nutritiva

    Directory of Open Access Journals (Sweden)

    José Lavres Junior

    2010-01-01

    Full Text Available The deleterious effects of Mn stress on many species have been studied, mainly concerning biochemical, physiological and growth parameters of plants. However, there are few studies relating the anatomical and ultrastructural changes in response to manganese (Mn nutritional disorders, This study examined the leaf ultrastructure of Mn-inefficient (IAC-15, Santa Rosa and Mn-efficient (IAC-Foscarin 31 soybean (Glycine max L. genotypes in response to three rates of Mn (0.5, 2 and 200 µmol L-1 in the nutrient solution. Symptoms of Mn deficiency developed 12 days after transplanting in IAC-15 and Santa Rosa, followed by IAC-Foscarin 31 on the 15th day. Only IAC-15 and Santa Rosa leaves showed symptoms of Mn toxicity. The Mn concentration in leaves ranged from 8.6 (deficiency to 886.3 mg kg-1 d.w. (toxicity. There were no changes either in stomata length or stomata number per unit of leaf surface. Cytoplasm disorganization was observed in IAC-15 under Mn-excess. In this case, the cytoplasm was amorphous, densely stained and extensively disorganized, with increased vacuolation. Mn effects were not found in mitochondria and nucleus in any of the genotypes tested. Under all Mn concentrations, many lipid globules were observed in the IAC15 chloroplasts. There was an increase in the number of plastids as well as in the size of starch grains within IAC-Foscarin 31 chloroplasts as Mn concentration in the nutrient solution increased. Genotypes had marked differences in the ultrastructure organization, mainly in leaf chloroplasts grown under conditions of both Mn deficiency and toxicity (the most sensitive genotype was IAC-15.Os efeitos negativos provocados tanto pela deficiência quanto pela toxidez de manganês (Mn no desenvolvimento das plantas têm sido avaliados, considerando-se os aspectos bioquímicos e produtivos da parte aérea, particularmente, onde os sintomas visuais são manifestados. Entretanto, há poucas informações na literatura abordando as

  1. Insect damage and powdery mildew severity in soybean cultivars and lines Danos de insetos e severidade de oídio em cultivares e linhagens de soja

    Directory of Open Access Journals (Sweden)

    André Luiz Lourenção

    2004-12-01

    Full Text Available The use of soybean cultivars resistant to insects and diseases reduces the application of pesticides, decreasing production costs and promoting a sustainable agriculture. The damage of stink bugs and defoliators and the severity of powdery mildew (Microsphaera diffusa in soybean of three maturity groups were evaluated under field conditions, at Tarumã and Ribeirão Preto, State of São Paulo, Brazil. Three experiments, one for each group, were carried out in the 1999/2000 and 2000/2001 growing seasons. In 1999/2000, the disease occurred in Tarumã; in that year, infestation of chrysomelids (Cerotoma sp. and Colaspis sp. was observed in Ribeirão Preto. Low infestations of stink bugs occurred in both years and locations, but in Tarumã, at the stage of plant maturation, the insect population exceeded the economic injury level. The severity of powdery mildew was evaluated using a scale varying from 1 (no symptom to 5 (more than 50% of leaves with symptoms. Chrysomelid injuries were estimated by the percentage of leaf area removed, and stink bug damage was evaluated by the percentage of leaf retention (LRP and yield. Within the early maturity group (110 days, IAC 94-2675 showed good yield levels, low LRP, and resistance to powdery mildew. In the genotypes of the 120-day maturity group, IAC 94-5, IAC 94-1172, IAC 94-1017, IAC 94-133, and IAC 94-745 presented good yield; the last two behaved as resistant to the disease. With regard to the genotypes of the 135-day maturity group, IAC 93-1564 and IAC 94-2939 showed good yield, low LRP, and resistance to powdery mildew.A utilização de cultivares de soja resistentes a pragas e doenças reduz a aplicação de pesticidas, diminuindo custos de produção e favorecendo uma agricultura sustentável. Assim, avaliaram-se os danos causados por percevejos e coleópteros crisomelídeos e a severidade de oídio (Microsphaera diffusa em cultivares e linhagens de soja de ciclos precoce, semiprecoce e médio, em

  2. Comparação entre cultivares de soja quanto à preferência alimentar de Cerotoma arcuata e suscetibilidade a um isolado do vírus do mosaico severo do caupi Comparison among soybean cultivars concerning the feed preference of Cerotoma arcuata and susceptibility to an isolate of CpSMV

    Directory of Open Access Journals (Sweden)

    Fernando Javier Sanhueza Salas

    1998-01-01

    Full Text Available Entre as viroses que causam prejuízos às culturas de leguminosas no Brasil, principalmente soja (Glycine max, feijão (Pliaseolus vulgaris e caupi (Vigna unguiculata, inclui-se o mosaico severo do caupi, "cowpea severe mosaic Comovirus" - CpSMV, transmitido por Cerotoma arcuata (Coleóptera; Chrysomelidae. Um isolado deste vírus, denominado CpSMV-SP, proveniente de plantas de Vigna luteola coletadas no litoral sul do Estado de São Paulo, está sendo estudado no Laboratório de Fitovirologia e Fisiopatologia/ Instituto Biológico. O objetivo do presente trabalho consistiu em uma avaliação da preferência alimentar de C. arcuata em cultivares de soja e da suscetibilidade destes cultivares ao vírus. Na avaliação da preferência alimentar, os ensaios foram feitos com discos foliares colocados em placas de Petri, cobertas por copos plásticos, constituindo "arenas". Introduziu-se um coleóptero em cada "arena", realizando-se testes em confinamento, tanto com múltipla escolha (11 cultivares como sem (um único cultivar. Os cultivares avaliados foram: 'BR-4', 'COODEPEC-201', 'EMBRAPA-48', 'EMBRAPA-59', 'IAC-177IAC-15-1', 'IAC-20', 'IAC-100', 'IAS-5', 'IGUAÇU' e 'PL-1'. Os ensaios de transmissão foram feitos através de inoculação mecânica e pelo vetor C. arcuata. Os resultados mostraram que os 11 cultivares são suscetíveis ao vírus, quando a inoculação é feita por extrato (mecanicamente. Ocorre também transmissão pelo coleóptero, porém não no caso de IAC-20 e IAC-100. C. arcuata alimenta-se de todos os cultivares, em maior ou em menor intensidade, exceção feita ao IAC-20, fato que pode justificar a não transmissão pelo menos para estas plantas. Considerando que a disseminação natural do CpSMV-SP ocorre através do vetor, e que ela é negativa para os dois cultivares referidos, pode-se recomendar preferencialmente o seu plantio, no Estado de São Paulo.In Brazil, among the viruses causing crop losses in leguminous plants

  3. Selectivity in microemulsion electrokinetic chromatography

    DEFF Research Database (Denmark)

    Pedersen-Bjergaard, S; Gabel-Jensen, Charlotte; Honoré Hansen, S

    2000-01-01

    Microemulsion electrokinetic chromatography (MEEKC) is a most promising separation technique providing good selectivity and high separation efficiency of anionic, cationic as well as neutral solutes. In MEEKC lipophilic organic solvents dispersed as tiny droplets in an aqueous buffer by the use...

  4. Compound immobilization and drug-affinity chromatography.

    Science.gov (United States)

    Rix, Uwe; Gridling, Manuela; Superti-Furga, Giulio

    2012-01-01

    Bioactive small molecules act through modulating a yet unpredictable number of targets. It is therefore of critical importance to define the cellular target proteins of a compound as an entry point to understanding its mechanism of action. Often, this can be achieved in a direct fashion by chemical proteomics. As with any affinity chromatography, immobilization of the bait to a solid support is one of the earliest and most crucial steps in the process. Interfering with structural features that are important for identification of a target protein will be detrimental to binding affinity. Also, many molecules are sensitive to heat or to certain chemicals, such as acid or base, and might be destroyed during the process of immobilization, which therefore needs to be not only efficient, but also mild. The subsequent affinity chromatography step needs to preserve molecular and conformational integrity of both bait compound and proteins in order to result in the desired specific enrichment while ensuring a high level of compatibility with downstream analysis by mass spectrometry. Thus, the right choice of detergent, buffer, and protease inhibitors is also essential. This chapter describes a widely applicable procedure for the immobilization of small molecule drugs and for drug-affinity chromatography with subsequent protein identification by mass spectrometry.

  5. First-line intra-arterial versus intravenous chemotherapy in unilateral sporadic group D retinoblastoma: evidence of better visual outcomes, ocular survival and shorter time to success with intra-arterial delivery from retrospective review of 20 years of treatment.

    Science.gov (United States)

    Munier, Francis L; Mosimann, Pascal; Puccinelli, Francesco; Gaillard, Marie-Claire; Stathopoulos, Christina; Houghton, Susan; Bergin, Ciara; Beck-Popovic, Maja

    2017-08-01

    The introduction of intra-arterial chemotherapy (IAC) as salvage treatment has improved the prognosis for eye conservation in group D retinoblastoma. The aim of this study was to compare the outcomes of consecutive patients with advanced unilateral disease treated with either first-line intravenous chemotherapy (IVC) or first-line IAC. This is a retrospective mono-centric comparative review of consecutive patients. Sporadic unilateral retinoblastoma group D cases treated conservatively at Jules-Gonin Eye Hospital and CHUV between 1997 and 2014. From January 1997 to August 2008, IVC, combined with focal treatments, was the primary treatment approach. From September 2008 to October 2014, IAC replaced IVC as first-line therapy. 48 patients met the inclusion criteria, receiving only either IAC or IVC as primary treatment modality. Outcomes of 23 patients treated by IVC were compared with those of 25 treated by IAC; mean follow-up was 105.3 months (range 29.2-218.6) and 41.7 months (range 19.6-89.5), respectively. Treatment duration was significantly shorter in the IAC group (pchemotherapy treatment. Despite this, the results reported here imply that eyes treated with first-line IAC will have shorter treatment period, better ocular survival and visual acuity than first-line IVC. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/.

  6. Resposta de genótipos de trigo à inoculação de bactérias diazotróficas em condições de campo Wheat genotypes response to inoculation of diazotrophic bacteria in field conditions

    Directory of Open Access Journals (Sweden)

    Valéria Marino Rodrigues Sala

    2007-06-01

    Full Text Available O objetivo deste trabalho foi avaliar, em condições de campo, o efeito e a viabilidade econômica da inoculação de novos isolados homólogos de bactérias diazotróficas endofíticas, sob diferentes doses de nitrogênio, em dois genótipos de trigo, em duas localidades. Foram utilizados: três isolados de bactérias diazotróficas endofíticas (IAC-AT-8, Azospirillum brasilense; IAC-HT-11, Achromobacter insolitus; IAC-HT-12, Zoogloea ramigera, dois genótipos de trigo (ITD-19 e IAC-370 e três doses de N, na forma de uréia (0, 60 e 120 kg ha-1. No estádio de quatro folhas e no perfilhamento, foram avaliados a massa de matéria seca e o N acumulado na parte aérea. Na colheita, foram avaliados o teor de N, a massa de 1.000 sementes e a produtividade de grãos. A inoculação promoveu maior massa de matéria seca e N acumulado e aumentou a produtividade de grãos, principalmente na presença de adubo nitrogenado, com lucro para o agricultor. Entretanto, o maior aumento na produtividade de grãos foi obtido nas plantas do genótipo IAC-370, com o emprego do isolado IAC-HT-12, na ausência de N, que superou em 45% o tratamento testemunha. As respostas variaram em relação ao local de cultivo, o que sugere expressiva interação planta-bactéria-ambiente.The aim of this work was to evaluate, in field conditions, the effect and the economic viability of inoculation of new homologous strains endophytic diazotrophic bacteria, under different nitrogen doses on two wheat genotypes. Three strains of diazotrophic bacteria (IAC-AT-8, Azospirillum brasilense; IAC-HT-11, Achromobacter insolitus; IAC-HT-12, Zoogloea ramigera, two wheat genotypes (ITD-19 and IAC-370, and three levels of nitrogen fertilizer as urea (0, 60 e 120 kg ha-1 were tested. Shoot dry matter and total shoot nitrogen were evaluated, at four leaves and at tillering stages. Nitrogen concentration in the grain, 1,000 grains weight and yield were evaluated at harvest. Plants with

  7. Use of micro gas chromatography in the fuel cycle of fusion reactors

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.; Kawamura, Y.

    2003-01-01

    Various analytical techniques exist to determine the compositions of gases handled in the fuel cycle of future fusion machines. Gas chromatography was found to be the most appropriate method. The main disadvantages of conventional gas chromatography were the long retention times for the heavy hydrogen species of >30 min. Recent progress in the development of micro-gas chromatography has reduced these retention times to ∼3 min. The usefulness of micro-gas chromatography for the analysis of hydrogen and impurity gas mixtures in the fuel cycle of future fusion machines is presented and the advantages and drawbacks are discussed

  8. Fabrication of Ceramic Membrane Chromatography for Biologics Purification

    Directory of Open Access Journals (Sweden)

    Maizirwan Mel

    2011-12-01

    Full Text Available Chromatography is one of the most important separation processes of choice for the recovery/purification of proteins and complex bio-structures. Fabrication of chromatographic membranes and their efficiency in the chromatography process has been the subject of many recent researches. In this study, a coin-like, 13 mm diameter and 3 mm thick, ceramic membrane was fabricated to be used as a chromatographic medium. The membrane is used to replace the conventional resin-based chromatography columns. Hydroxyapatite (HA powder was used as a material for the membrane fabrication. In this project, a HA powder was produced using starch as pore creating agents. Characterization processes were done for the ceramic membrane using the suitable apparatuses. Three parameters of the fabrication process (starch wt %, compaction pressure and sintering temperature were manipulated to optimize the performance of the membrane. The fabricated membrane was placed in a (FPLC system to be tested for its performance as an adsorptive membrane. (IMAC process was run by immobilizing Ni2+ ions at the membrane particles surfaces. NP protein of the (NDV was used to test the membrane's ability to bind Histidine-tagged proteins. The optimum set of process parameters that yielded in the highest porosity and good chromatogram was determined to be 5 wt % starch, 3000 psi compaction pressure and 1100°C sintering temperature.ABSTRAK: Kromatografi merupakan satu daripada proses pengasingan yang penting yang dipilih untuk perolehan/penapisan protein dan biostruktur yang kompleks. Pemfabrikatan membran kromatografi dan kecekapannya dalam proses kromatografi merupakan fokus beberapa kajian terkini. Dalam kajian ini, membran seramik berbentuk duit syiling, berdiameter 13 mm dengan ketebalan 3 mm, direka untuk digunakan sebagai perantara kromatografi. Membran ini digunakan untuk menggantikan turus kromatografi berasaskan resin yang lazim. Serbuk hidroksiapatit (HA digunakan sebagai bahan

  9. Study of radiolysis products of natural organic materials by means of gas chromatography

    International Nuclear Information System (INIS)

    Pogocki, D.

    1994-01-01

    Analytical methods based on gas chromatography for identification determination of products arising during food irradiation have been presented. Behind the classics version of the methods one has shown also combined methods being the on-line connection of gas chromatography with mass spectroscopy as well as gas chromatography with liquid chromatography and mass spectroscopy. The applicability as well as weakness and advantages of each version have been discussed on the context of food irradiation. 11 refs, 7 figs

  10. Integrated sampling vs ion chromatography: Mathematical considerations

    International Nuclear Information System (INIS)

    Sundberg, L.L.

    1992-01-01

    This paper presents some general purpose considerations that can be utilized when comparisons are made between the results of integrated sampling over several hours or days, and ion chromatography where sample collection times are measured in minutes. The discussion is geared toward the measurement of soluble transition metal ions in BWR feedwater. Under steady-state conditions, the concentrations reported by both techniques should be in reasonable agreement. Transient operations effect both types of measurements. A simplistic model, applicable to both sampling techniques, is presented that demonstrates the effect of transients which occur during the acquisition of a steady-state sample. For a common set of conditions, the integrated concentration is proportional to the concentration and duration of the transient, and inversely proportional to the sample collection time. The adjustment of the collection period during a known transient allows an estimation of peak transient concentration. Though the probability of sampling a random transient with the integrated sampling technique is very high, the magnitude is severely diluted with long integration times. Transient concentrations are magnified with ion chromatography, but the probability of sampling a transient is significantly lower using normal ion chromatography operations. Various data averaging techniques are discussed for integrated sampling and IC determinations. The use of time-weighted averages appears to offer more advantages over arithmetic and geometric means for integrated sampling when the collection period is variable. For replicate steady-state ion chromatography determinations which bracket a transient sample, it may be advantageous to ignore the calculation of averages, and report the data as trending information only

  11. DIRECT-DEPOSITION INFRARED SPECTROMETRY WITH GAS AND SUPERCRITICAL FLUID CHROMATOGRAPHY

    Science.gov (United States)

    A direct-deposition Fourier transform infrared (FT-IR) system has been evaluated for applicability to gas chromatography (GC) and supercritical fluid chromatography (SFC) of environmental analytes. A 100-um i.d. fused-silica transfer line was used for GC, and a 50-um transfer lin...

  12. Liquid phase chromatography on microchips

    DEFF Research Database (Denmark)

    Kutter, Jörg Peter

    2012-01-01

    explosive development of, in particular, chromatographic separation systems on microchips, has, however, slowed down in recent years. This review takes a closer, critical look at how liquid phase chromatography has been implemented in miniaturized formats over the past several years, what is important...

  13. Separation of Aeruginosin-865 from Cultivated Soil Cyanobacterium (Nostoc sp.) by Centrifugal Partition Chromatography combined with Gel Permeation Chromatography.

    Science.gov (United States)

    Cheel, José; Minceva, Mirjana; Urajová, Petra; Aslam, Rabya; Hrouzek, Pavel; Kopecký, Jiří

    2015-10-01

    Aeruginosin-865 was isolated from cultivated soil cyanobacteria using a combination of centrifugal partition chromatography (CPC) and gel permeation chromatography. The solubility of Aer-865 in different solvents was evaluated using the conductor-like screening model for real solvents (COSMO-RS). The CPC separation was performed in descending mode with a biphasic solvent system composed of water-n-BuOH-acetic acid (5:4:1, v/v/v). The upper phase was used as a stationary phase, whereas the lower phase was employed as a mobile phase at a flow rate of 10 mL/min. The revolution speed and temperature of the separation column were 1700 rpm and 25 degrees C, respectively. Preparative CPC separation followed by gel permeation chromatography was performed on 50 mg of crude extract yielding Aer-865 (3.5 mg), with a purity over 95% as determined by HPLC. The chemical identity of the isolated compound was confirmed by comparing its spectroscopic data (UV, HRESI-MS, HRESI-MS/MS) with those of an authentic standard and data available in the literature.

  14. Ultra-high Performance Liquid Chromatography in Steroid Analysis

    OpenAIRE

    Salonen, Fanny

    2017-01-01

    The latest version of liquid chromatography is ultra-high performance (or pressure) chromatography (UHPLC). In the technique, short and narrow-bore columns with particle sizes below 3 µm are used. The extremely high pressure used results in very short analysis times, excellent separation, and good resolution. This makes UHPLC a good choice for steroidal analysis. Steroids are a highly interesting area of study; they can be recognized as biomarkers for several diseases and are a relevant topic...

  15. Gas chromatography of β-diketonates

    International Nuclear Information System (INIS)

    Burgett, C.A.

    1976-01-01

    The history of separation of metal complexes by gas chromatography is reviewed. The greatest success has been achieved with metal halides or metal β-diketonates, particularly with chelates of the small elements, Be and Al, and the extremely inert chromium diketonates. Many problems still remain concerning the development of suitable chromatographic techniques for many chelates; however, the technique of synergic solvent extraction, mixed-ligand complex chromatography, the synthesis of new heteroatomic ligands, and the advent of new liquid phases are discussed as means to increase the number of unique techniques for separation and analysis of metals. Methods are suggested and references are cited for chromatographic analysis of elements in the following groups: alkali metals, alkaline earths, Group IIIA, IVB, VB, VIB, VIIB, VIII, IB, and IIB. Special attention is given to separation of the volatile complexes of Sc, Y, the lanthanides, the actinides, and Pb. 156 references

  16. Lipidomics by Supercritical Fluid Chromatography

    Directory of Open Access Journals (Sweden)

    Laurent Laboureur

    2015-06-01

    Full Text Available This review enlightens the role of supercritical fluid chromatography (SFC in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC. It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering or highly specific (mass spectrometry detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides defined by the LIPID MAPS consortium.

  17. Lipidomics by Supercritical Fluid Chromatography

    Science.gov (United States)

    Laboureur, Laurent; Ollero, Mario; Touboul, David

    2015-01-01

    This review enlightens the role of supercritical fluid chromatography (SFC) in the field of lipid analysis. SFC has been popular in the late 1980s and 1990s before almost disappearing due to the commercial success of liquid chromatography (LC). It is only 20 years later that a regain of interest appeared when new commercial instruments were introduced. As SFC is fully compatible with the injection of extracts in pure organic solvent, this technique is perfectly suitable for lipid analysis and can be coupled with either highly universal (UV or evaporative light scattering) or highly specific (mass spectrometry) detection methods. A short history of the use of supercritical fluids as mobile phase for the separation oflipids will be introduced first. Then, the advantages and drawbacks of SFC are discussed for each class of lipids (fatty acyls, glycerolipids, glycerophospholipids, sphingolipids, sterols, prenols, polyketides) defined by the LIPID MAPS consortium. PMID:26090714

  18. WHEAT CULTIVARS: RESPONSE TO IRRIGATION AND SOWING DATES

    Directory of Open Access Journals (Sweden)

    Klar A.E.

    1996-01-01

    Full Text Available This study was carried out in an Alfisol-Oxisol transition sandy-clay texture, using six wheat cultivars (Triticum aestivum, L.: two tall and tolerant to soil aluminium toxicity (BH-1146, and IAC-18, and four semi-dwarf cultivars - Anahuac, IAC-162, IAC-24, and IAC-60 - of which only the first two are sensitive to soil aluminium toxicity. Two minimum soil water potentials (ys levels were used: 1. watered, when Ys reached about -0.05 MPa; 2. dry, when the water potential reached around -1.5 MPa. Two sowing dates, 05/22/92 and 06/11/92, were used. The results showed that Anahuac and IAC-60 are the most indicated cultivars for the studied region; when irrigated all cultivars presented similar yield level under no irrigation conditions; the irrigation was not sufficient to avoid yield differences between the two growing seasons; differences in rainfall were important for the crop in the dry treatment for both seasons.

  19. Applications of hydrophilic interaction chromatography to amino acids, peptides, and proteins.

    Science.gov (United States)

    Periat, Aurélie; Krull, Ira S; Guillarme, Davy

    2015-02-01

    This review summarizes the recent advances in the analysis of amino acids, peptides, and proteins using hydrophilic interaction chromatography. Various reports demonstrate the successful analysis of amino acids under such conditions. However, a baseline resolution of the 20 natural amino acids has not yet been published and for this reason, there is often a need to use mass spectrometry for detection to further improve selectivity. Hydrophilic interaction chromatography is also recognized as a powerful technique for peptide analysis, and there are a lot of papers showing its applicability for proteomic applications (peptide mapping). It is expected that its use for peptide mapping will continue to grow in the future, particularly because this analytical strategy can be combined with reversed-phase liquid chromatography, in a two-dimensional setup, to reach very high resolving power. Finally, the interest in hydrophilic interaction chromatography for intact proteins analysis is less evident due to possible solubility issues and a lack of suitable hydrophilic interaction chromatography stationary phases. To date, it has been successfully employed only for the characterization of membrane proteins, histones, and the separation of glycosylated isoforms of an intact glycoprotein. From our point of view, the number of hydrophilic interaction chromatography columns compatible with intact proteins (higher upper temperature limit, large pore size, etc.) is still too limited. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Ophthalmic Vascular Events after Primary Unilateral Intra-arterial Chemotherapy for Retinoblastoma in Early and Recent Eras.

    Science.gov (United States)

    Dalvin, Lauren A; Ancona-Lezama, David; Lucio-Alvarez, J Antonio; Masoomian, Babak; Jabbour, Pascal; Shields, Carol L

    2018-06-16

    To assess risk factors for ophthalmic vascular events after intra-arterial chemotherapy (IAC) for retinoblastoma. Retrospective cohort study. Patients who received unilateral IAC as primary treatment for retinoblastoma from January 1, 2009, to November 30, 2017, at a single center. Records were reviewed for patient demographics, tumor features, IAC parameters, and treatment-related vascular events in the early IAC era (2009-2011) compared with the recent era (2012-2017) using the t test and Fisher exact test. Change in event rates over time was assessed using Poisson regression analysis, with Spearman's rho used to test correlation. Rate of IAC-induced ophthalmic vascular events. There were 243 chemotherapy infusions in 76 eyes of 76 patients, divided into early (22 eyes, 57 infusions) and recent (54 eyes, 186 infusions) eras. Intra-arterial chemotherapy consisted of melphalan (243 infusions), topotecan (124 infusions), and carboplatin (9 infusions). A comparison (early vs. recent era) revealed fewer mean number of infusions (2.6 vs. 3.4, P = 0.02) with similar mean patient age and presenting tumor features. Event rates decreased over time (P early era vs. recent era) in the recent era (59% vs. 9% per eye, 23% vs. 3% per infusion, P age (P = 0.75), tumor diameter (P = 0.32), tumor thickness (P = 0.59), or cumulative dosage of melphalan (P = 0.13) or topotecan (P = 0.59). There were no IAC-induced vascular events in 72 infusions of 21 consecutively treated eyes in 2016 to 2017. Ophthalmic vascular events after IAC have decreased from the early era (2009-2011) through the current era (2012-2017) at this center. Experience performing this highly specialized procedure could be an important factor predicting IAC-related vascular events. Copyright © 2018 American Academy of Ophthalmology. Published by Elsevier Inc. All rights reserved.

  1. Estudo comparativo de cultivares de trigo em latossolo roxo no estado de São Paulo em 1974 A comparative study on wheat cultivars on latossolic B "Terra Roxa" soils in the state of São Paulo in 1974

    Directory of Open Access Journals (Sweden)

    João Carlos Felício

    1976-01-01

    Full Text Available Este trabalho foi executado com o propósito de estudar o comportamento de diferentes cultivares de trigo, em latossolo roxo na região tritícola do Vale do Paranapanema no Estado de São Paulo. Foram instalados três experimentos em 1974. Os cultivares IRN-526-63, IAS-55, Sonora-63, BH-1146, IAS-54, Londrina, LA-1434 e Pitic-62 foram os que apresentaram maior produtividade por unidade de área; os cultivares IAC-5, Sonora-63, Sonora-64 x Selkirk, Triticum agropyrum, Tobari-66, IAC-11, Sonora-64, Norteno-67 e Super X mostraram-se resistentes às raças prevalentes de ferrugem do colmo. Os cultivares Super X, Sonora-64 x Selkirk, IRN-152-63 e Triticum agropyrum mostraram-se resistentes à ferrugem da folha, e BH-1146, IAC-5, IAC-11, LA-1434, T. agropyrum e IRN-152-63 foram suscetíveis ao acamamento.Selected germplasms of wheat were tested for yield potential and resistance to rusts and cultivar trials in the State of São Paulo. Performance was evaluated in several locations in 1974 in the wheat area of the State on Latossolic B "Terra Roxa" soils. The cultivars IRN-526-63, IAS-55, Sonora-63, BH-1146, IAS-54, Londrina, LA-1434 and Pitic-62 showed superior performance for yield. The cultivars IAC-5, Sonora-63, Sonora-64 x Selkink, Triticum agropyrum, Tobai-66, IAC-11, Sonora-64, Norteno-67, and Super X showed better resistance to stem rust. The cultivars Super X, Sonora-64 x Selkink, IRN-152,63, and Triticum agropyrum, were more resistant to leaf rust. The cultivars BH-1146, IAC-5, Triticum agropyrum, IRN-152-62, LA-1434 and IAC-11 were susceptible to lay.

  2. Using Ion Exchange Chromatography to Separate and Quantify Complex Ions

    Science.gov (United States)

    Johnson, Brian J.

    2014-01-01

    Ion exchange chromatography is an important technique in the separation of charged species, particularly in biological, inorganic, and environmental samples. In this experiment, students are supplied with a mixture of two substitution-inert complex ions. They separate the complexes by ion exchange chromatography using a "flash"…

  3. Use and practice of achiral and chiral supercritical fluid chromatography in pharmaceutical analysis and purification.

    Science.gov (United States)

    Lemasson, Elise; Bertin, Sophie; West, Caroline

    2016-01-01

    The interest of pharmaceutical companies for complementary high-performance chromatographic tools to assess a product's purity or enhance this purity is on the rise. The high-throughput capability and economic benefits of supercritical fluid chromatography, but also the "green" aspect of CO2 as the principal solvent, render supercritical fluid chromatography very attractive for a wide range of pharmaceutical applications. The recent reintroduction of new robust instruments dedicated to supercritical fluid chromatography and the progress in stationary phase technology have also greatly benefited supercritical fluid chromatography. Additionally, it was shown several times that supercritical fluid chromatography could be orthogonal to reversed-phase high-performance liquid chromatography and could efficiently compete with it. Supercritical fluid chromatography is an adequate tool for small molecules of pharmaceutical interest: synthetic intermediates, active pharmaceutical ingredients, impurities, or degradation products. In this review, we first discuss about general chromatographic conditions for supercritical fluid chromatography analysis to better suit compounds of pharmaceutical interest. We also discuss about the use of achiral and chiral supercritical fluid chromatography for analytical purposes and the recent applications in these areas. The use of preparative supercritical fluid chromatography by pharmaceutical companies is also covered. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. EVALUATING THE FRUIT PRODUCTION AND QUALITY OF CHERRY TOMATO (Solanum lycopersicum var. cerasiforme EVALUACIÓN DE LA PRODUCCIÓN Y CALIDAD DEL FRUTO DEL TOMATE CEREZA Solanum lycopersicum var. cerasiforme

    Directory of Open Access Journals (Sweden)

    Nelson Ceballos Aguirre

    2012-06-01

    Full Text Available Abstract. The greatest genetic diversity of tomato (Solanum lycopersicum L. in terms of fruit quality characteristics such as flavor, aroma, color, and lycopene and b-carotene contents is found in wild species. This study evaluated the agronomic characteristics and fruit quality of 30 cherry tomato introductions of the germplasm bank of the Universidad Nacional de Colombia - Sede Palmira in trials conducted at the Montelindo experimental farm of the Universidad de Caldas (1010 m above sea level, average temperature 22.8 °C, average annual rainfall 2200 mm, 76% relative humidity. A 5 x 6 rectangular lattice experimental design was used with 30 treatments (introductions and a commercial control (Sweet Million, 4 replicates/treatment, and 5 plants/replicate as experimental unit. The descriptors used were those suggested by the former International Plant Genetic Resources Institute, now Bioversity International. Data were statistically analyzed by ANOVA and Duncan's means test using the SAS program. In addition, principal component and cluster dendrogram analyses using the SAS Princom and Cluster procedure (SAS Institute, Cary, NC were performed. Six principal components accounted for 80.39% of the morphological variability of the introductions evaluated. The most promising materials in terms of average fruit weight, yield per plant and per hectare, and soluble solids, vitamin C and lycopene contents were IAC1624, IAC391, IAC3652, LA2131, IAC424, IAC1621, IAC426, LA1480 and IAC1688. The broad phenotypic variability observed in the evaluated introductions favors the potential selection and breeding of tomato for traits associated with fruit production and quality.Resumen. La mayor diversidad genética del tomate (Solanum lycopersicum L. en términos de características de calidad del fruto como sabor, aroma, coloración y contenidos de licopeno y b-caroteno se encuentra en especies silvestres. Este estudio evaluó las características agronómicas y

  5. Tolerância de genótipos de trigo comum, trigo duro e triticale à toxicidade de alumínio em soluções nutritivas Tolerance of bread wheat, durum wheat and triticale genotypes to aluminum toxicity in nutrient solution

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo de Oliveira Camargo

    2006-01-01

    Full Text Available Foi estudado o comportamento diferencial de 12 genótipos de trigo comum (Triticum aestivum L., um genótipo de trigo duro (Triticum durum L., e um de triticale (Triticosecale sp em soluções nutritivas de tratamento contendo duas concentrações salinas (1/5 e 1/10 da completa e seis concentrações de alumínio ( 0, 2, 4, 6, 8 e 10 mg L-1, à temperatura de 25 ± 1ºC e pH 4,0. Foram utilizadas dez plântulas por parcela e quatro repetições. A tolerância foi medida pela capacidade de as raízes primárias continuarem a crescer em solução sem alumínio, após permanecer 48 horas em solução nutritiva completa, contendo uma concentração conhecida de alumínio combinada com cada uma das concentrações salinas. Os genótipos de trigo comum IAC-289, IAC-350 e IAC-370 e a cultivar controle Anahuac, e os genótipos de trigo duro IAC-1003 e de triticale IAC-5 foram os mais sensíveis a níveis crescentes de Al3+nas soluções nutritivas de tratamento e, portanto, somente seriam indicados para cultivo em solos corrigidos. Os genótipos de trigo comum IAC-24 e IAC-378 e a cultivar controle BH-1146 destacaram-se pela tolerância à toxicidade de Al3+, com potencial para uso em solos ácidos e como fontes genéticas de tolerância nos futuros cruzamentos. Os sintomas de toxicidade de alumínio foram maiores com a elevação da concentração de alumínio e da diminuição das concentrações de sais da solução nutritiva para todos os genótipos estudados.Twelve bread wheat (Triticum aestivum L., one durum wheat (Triticum durum L. and one triticale (Triticosecale sp genotypes were studied in nutrient solutions with a high salt concentration in experiment 1 and a weak salt concentration in experiment 2, for aluminum tolerance at six levels: 0, 2, 4, 6, 8 and 10 mg L-1, under temperature 25 ± 1ºC and pH 4,0. Four replications were used per experiment. Aluminum tolerance was evaluated by measuring root growth in an aluminum-free complete

  6. Spillage detector for liquid chromatography systems

    Science.gov (United States)

    Jarvis, M. J.; Fulton, D. S. (Inventor)

    1986-01-01

    A spillage detector device for use in conjunction with fractionation of liquid chromatography systems which includes a spillage recieving enclosure beneath the fractionation area is described. A sensing device having a plurality of electrodes of alternating polarity is mounted within the spillage recieving enclosure. Detection circuitry, responsive to conductivity between electrodes, is operatively connected to the sensing device. The detection circuitry feeds into the output circuitry. The output circuit has relaying and switching circuitry directed to a solenoid, an alarm system and a pump. The solenoid is connected to the pliable conduit of the chromatography system. The alarm system comprises an audio alarm and a visual signal. A 115-volt power system interconnected with the pump, the solenoid, the sensing device, and the detection and output circuitry.

  7. Narrow, duplicated internal auditory canal

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, T. [Servico de Neurorradiologia, Hospital Garcia de Orta, Avenida Torrado da Silva, 2801-951, Almada (Portugal); Shayestehfar, B. [Department of Radiology, UCLA Oliveview School of Medicine, Los Angeles, California (United States); Lufkin, R. [Department of Radiology, UCLA School of Medicine, Los Angeles, California (United States)

    2003-05-01

    A narrow internal auditory canal (IAC) constitutes a relative contraindication to cochlear implantation because it is associated with aplasia or hypoplasia of the vestibulocochlear nerve or its cochlear branch. We report an unusual case of a narrow, duplicated IAC, divided by a bony septum into a superior relatively large portion and an inferior stenotic portion, in which we could identify only the facial nerve. This case adds support to the association between a narrow IAC and aplasia or hypoplasia of the vestibulocochlear nerve. The normal facial nerve argues against the hypothesis that the narrow IAC is the result of a primary bony defect which inhibits the growth of the vestibulocochlear nerve. (orig.)

  8. Choices of capture chromatography technology in antibody manufacturing processes.

    Science.gov (United States)

    DiLeo, Michael; Ley, Arthur; Nixon, Andrew E; Chen, Jie

    2017-11-15

    The capture process employed in monoclonal antibody downstream purification is not only the most critically impacted process by increased antibody titer resulting from optimized mammalian cell culture expression systems, but also the most important purification step in determining overall process throughput, product quality, and economics. Advances in separation technology for capturing antibodies from complex feedstocks have been one focus of downstream purification process innovation for past 10 years. In this study, we evaluated new generation chromatography resins used in the antibody capture process including Protein A, cation exchange, and mixed mode chromatography to address the benefits and unique challenges posed by each chromatography approach. Our results demonstrate the benefit of improved binding capacity of new generation Protein A resins, address the concern of high concentration surge caused aggregation when using new generation cation exchange resins with over 100mg/mL binding capacity, and highlight the potential of multimodal cation exchange resins for capture process design. The new landscape of capture chromatography technologies provides options to achieve overall downstream purification outcome with high product quality and process efficiency. Copyright © 2017 Elsevier B.V. All rights reserved.

  9. Radioanalytical determination of plutonium and americium using ion exchange and extraction chromatography technique in urine

    International Nuclear Information System (INIS)

    Santhanakrishnan, V.; Sreedevi, K.R.; Rajaram, S.; Ravi, P.M.

    2011-01-01

    The use of anion exchange chromatography for the separation of Pu and extraction chromatography technique for the separation of Am from urine samples was studied. In the earlier method, Pu separation was carried out by anion exchange chromatography followed by Am separation by cation exchange chromatography. The chemical recovery of Am obtained by cation exchange separation method was inconsistent and low in the range 30-70%. In this study, the average Pu recovery obtained using anion exchange chromatography was 89.2 with standard deviation of 10.4 and the average Am recovery obtained using extraction chromatography with TRU resin was 77.4 with standard deviation of 14.8. Moreover, Am separation could be completed within three hours using the TRU column compared to two days that were required for the cation exchange chromatography. (author)

  10. Antixenosis of bean genotypes to Chrysodeixis includens (Lepidoptera: Noctuidae

    Directory of Open Access Journals (Sweden)

    Rafaela Morando

    2015-06-01

    Full Text Available The objective of this work was to evaluate bean genotypes for resistance to soybean looper (Chrysodeixis includens. Initially, free-choice tests were carried out with 59 genotypes, divided into three groups according to leaf color intensity (dark green, light green, and medium green, in order to evaluate oviposition preference. Subsequently, 12 genotypes with high potential for resistance were selected, as well as two susceptible commercial standards. With these genotypes, new tests were performed for oviposition in a greenhouse, besides tests for attractiveness and consumption under laboratory conditions (26±2ºC, 65±10% RH, and 14 h light: 10 h dark photophase. In the no-choice test with adults, in the greenhouse, the 'IAC Jabola', Arcelina 1, 'IAC Boreal', 'Flor de Mayo', and 'IAC Formoso' genotypes were the least oviposited, showing antixenosis-type resistance for oviposition. In the free-choice test with larvae, Arcelina 4, 'BRS Horizonte', 'Pérola', H96A102-1-1-1-52, 'IAC Boreal', 'IAC Harmonia', and 'IAC Formoso' were the less consumed genotypes, which indicates antixenosis to feeding. In the no-choice test, all genotypes (except for 'IAPAR 57' expressed moderate levels of antixenosis to feeding against C. includens larvae.

  11. Photoinduced Charge Transport Spectra for Porphyrin and Naphthalene Derivative-based Dendrimers

    Science.gov (United States)

    Park, J. H.; Wu, Y.; Parquette, J. R.; Epstein, A. J.

    2006-03-01

    Dendrimers are important chemical structures for harvesting charge. We prepared model dendrimers using two porphyrin derivatives and a naphthalene derivative. Films of these porphyrin derivatives have a strong Soret band (˜430nm) and four significant Q-bands; the naphthalene derivative has strong absorption at 365 and 383nm. Two kinds of photovoltaic cell structures [ITO/BaytronP/(thick or thin) dendrimer/Al] are constructed to investigate the optical response spectra of dendrimers under electric potential(V) on the cell (range from -1V to 2V). To obtain pure optical responses, incident light is modulated with an optical chopper and a lock-in amplifier is used to measure current (IAC) and phase (θ). For the excitation of the Soret band, IAC and θ do not change substantially with change of sign and amplitude of V. For Q-bands and naphthalene absorption bands, θ nearly follows the polarity of V on the cells and IAC is linear with V. Hence, IAC is nearly ohmic for Q- band although there are shifts due to built-in-potential. IAC for Soret band is almost same for thick and thin active layer cells. In contrast, IAC increases with thickness increase for Q bands. Mechanisms of photogeneration and charge transport will be discussed.

  12. A case of autoimmune cholangitis misdiagnosed for cholangiocarcinoma: How to avoid unnecessary surgical intervention?

    Directory of Open Access Journals (Sweden)

    Ignjatović Igor I.

    2015-01-01

    Full Text Available Introduction. Autoimmune cholangitis or immunoglobulin G4-associated cholangitis (IAC has been recently regarded as a new clinical and histopathological entity and is a part of a complex autoimmune disorder - IgG4-related systemic disease (ISD. ISD is an autoimmune disease with multi-organic involvement, characterized with IgG4-positive plasmocytic infiltration of various tissues and organs with a consequent sclerosis, which responds well to steroid therapy. Most commonly affected organs are the pancreas (autoimmune pancreatitis, [AIP] and the common bile duct (IAC. IAC and cholangiocarcinoma (CCA share many clinical, laboratory and imaging findings. Case Outline. We present a case of a 60-year-old male with a biliary stricture of a common bile duct, which was clinically considered as a bile duct carcinoma and treated surgically. Definite histopathological findings and immunohistochemistry revealed profound chronic inflammation, showing lymphoplasmacytic IgG-positive infiltration of a resected part of a common bile duct, highly suggestive for the diagnosis of IAC. In addition, postoperative IgG4 serum levels were also increased. Conclusion. It is of primary clinical importance to make a difference between IAC and CCA, in order to avoid unnecessary surgical intervention. Therefore, IAC should be considered in differential diagnosis in similar cases.

  13. The investigation of copper-based impregnated activated carbons prepared from water-soluble materials for broad spectrum respirator applications

    International Nuclear Information System (INIS)

    Smith, J.W.H.; Westreich, P.; Abdellatif, H.; Filbee-Dexter, P.; Smith, A.J.; Wood, T.E.; Croll, L.M.; Reynolds, J.H.; Dahn, J.R.

    2010-01-01

    The preparation of impregnated activated carbons (IACs) from aqueous, copper-containing solutions for broad spectrum gas filtration applications is studied here. Several samples were studied to determine the effect that impregnant loading, impregnant distribution and impregnant recipe had on the overall performance. Dynamic flow testing was used to determine the gas filtration capacity of the IAC samples versus a variety of challenge gases. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) were used to characterize the impregnant distribution on the carbon as a function of impregnant loading. Oven tests were performed to determine the thermal stability of the IAC samples exposed to elevated temperatures. The role impregnant distribution plays in gas filtration capacity and the overall performance of the IAC samples is discussed. The IAC samples prepared in this work were found to have gas filtration capacities as good as or better than broad spectrum respirator carbon samples prepared from the patent literature. IACs impregnated with an aqueous 2.4 M Cu(NO 3 ) 2 /0.04 M H 3 PO 4 .12MoO 3 /4 M HNO 3 solution that were heated to 200 deg. C under argon were found to have the best overall performance of the samples studied in this work.

  14. MRI enhancement of the facial nerve with Gd-DTPA, 2; Investigation of enhanced nerve portions in patients with facial palsy

    Energy Technology Data Exchange (ETDEWEB)

    Yanagida, Masahiro (Kansai Medical School, Moriguchi, Osaka (Japan))

    1993-08-01

    We performed enhanced MRI using Gd-DTPA in 84 patients with facial palsy. After assessing enhancement of the normal facial nerve, we examined enhancement in patients with Bell's palsy and Ramsay Hunt syndrome. In 95% of patients with Bell's palsy, enhancement was obtained in the distal IAC and labyrinthine portions. In 72%, enhancement was significant from the distal IAC portion through the vertical portion. In some of the patients who underwent enhanced MRI twice, increased signal intensity was observed in distal portions such as the vertical portion. In many cases of Ramsay Hunt syndrome, enhancement was seen extensively in the IAC portion through the vertical portion. In the subjects with internal auditory symptoms such as vertigo and tinnitus, enhancement of the IAC portion was seen not only in the facial nerve but also in the vestibular and the cochlear nerves. These results suggest that the vascular permeability of lesions in Bell's palsy may be increased from the distal IAC portion to the vertical portion. Judging from the present findings with Ramsay Hunt syndrome, symptoms related to the enhanced portions suggest that accompanying internal auditory symptoms occur due to inflammation of the IAC portions of cochlear and vestibular nerves. (author).

  15. Feasibility of correlating separation of ternary mixtures of neutral analytes via thin layer chromatography with supercritical fluid chromatography in support of green flash separations.

    Science.gov (United States)

    Ashraf-Khorassani, M; Yan, Q; Akin, A; Riley, F; Aurigemma, C; Taylor, L T

    2015-10-30

    Method development for normal phase flash liquid chromatography traditionally employs preliminary screening using thin layer chromatography (TLC) with conventional solvents on bare silica. Extension to green flash chromatography via correlation of TLC migration results, with conventional polar/nonpolar liquid mixtures, and packed column supercritical fluid chromatography (SFC) retention times, via gradient elution on bare silica with a suite of carbon dioxide mobile phase modifiers, is reported. Feasibility of TLC/SFC correlation is individually described for eight ternary mixtures for a total of 24 neutral analytes. The experimental criteria for TLC/SFC correlation was assumed to be as follows: SFC/UV/MS retention (tR) increases among each of the three resolved mixture components; while, TLC migration (Rf) decreases among the same resolved mixture components. Successful correlation of TLC to SFC was observed for most of the polar organic solvents tested, with the best results observed via SFC on bare silica with methanol as the CO2 modifier and TLC on bare silica with a methanol/dichloromethane mixture. Copyright © 2015 Elsevier B.V. All rights reserved.

  16. Evaluation of Continuous Membrane Chromatography Concepts with an Enhanced Process Simulation Approach

    Directory of Open Access Journals (Sweden)

    Steffen Zobel-Roos

    2018-03-01

    Full Text Available Modern biopharmaceutical products strive for small-scale, low-cost production. Continuous chromatography has shown to be a promising technology because it assures high-capacity utilization, purity and yield increases, and lower facility footprint. Membrane chromatography is a fully disposable low-cost alternative to bead-based chromatography with minor drawbacks in terms of capacity. Hence, continuous membrane chromatography should have a high potential. The evaluation of continuous processes goes often along with process modeling. Only few experiments with small feed demand need to be conducted to estimate the model parameters. Afterwards, a variety of different process setups and working points can be analyzed in a very short time, making the approach very efficient. Since the available modeling approaches for membrane chromatography modules did not fit the used design, a new modeling approach is shown. This combines the general rate model with an advanced fluid dynamic distribution. Model parameter determination and model validation were done with industrial cell cultures containing Immunoglobulin G (IgG. The validated model was used to evaluate the feasibility of the integrated Counter Current Chromatography (iCCC concept and the sequential chromatography concept for membrane adsorber modules, starting with a laboratory-type module used for sample preparation. A case study representing a fed-batch reactor with a capacity from 20 to 2000 L was performed. Compared to batch runs, a 71% higher capacity, 48.5% higher productivity, and 38% lower eluent consumption could be achieved.

  17. Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

    Science.gov (United States)

    Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

    2017-11-24

    Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

  18. The compactness of front tracking for chromatography electrophoresis and incompressible multiphase flow

    International Nuclear Information System (INIS)

    Wendroff, B.

    1992-01-01

    An analysis of the equations of chromatography from the point of view of hyperbolic conservation laws has been reviewed in recent literature. Serre was able to prove that the Lax-Friedrichs difference scheme, Godunov's method, and the viscosity method, have a subsequence converging to a weak solution of the chromatography equations, with no restriction on the size of the initial data. The purpose of this note is to announce that two versions of front tracking can be added to this list. After a brief description of the properties of the chromatography system and a definition of front tracking we give the basic steps of the proof. An example showing the quality of a front tracking solution is given. The equations of idealized electrophoresis and multiphase incompressible flow are very similar to the chromatography equations, but the former have linearly degenerate characteristic field, creating contact discontinuities. In the final section we briefly indicate how our result for chromatography carries over to this case

  19. Ion-pair chromatography of nucleic acid derivatives

    International Nuclear Information System (INIS)

    Perrone, P.A.; Brown, P.R.

    1985-01-01

    Little work has been done on the ion-pair chromatography of nucleic acid constituents, although there is a great potential for the use of this technique in the field. Since the classic work in 1949, nucleotides, as well as nucleosides and bases, have been separated by ion-exchange chromatography. However, ion exchange is a difficult mode and most researchers prefer the use of reversed-phase whenever possible. Although reversed-phase is now the method of choice, ionic compounds like nucleotides and some of the more polar bases are not adequately retained by many systems of this type. In addition, it is difficult to analyze simultaneously members of all three classes of nucleic acid compounds (bases, nucleosides, and nucleotides) using a reversed-phase system, even with gradient elution. Ion pairing can be a useful technique because, theoretically, the separation of nonionic bases and nucleosides along with the ionic nucleotides can be achieved. Additionally, each group of compounds may be separated isocratically. In this chapter, they will discuss ion-pair chromatography as applied to nucleic acid constituents. The current theories, advantages and disadvantages, a limited number of applications, and potential for future work are presented

  20. Expanded-bed chromatography in primary protein purification.

    Science.gov (United States)

    Anspach, F B; Curbelo, D; Hartmann, R; Garke, G; Deckwer, W D

    1999-12-31

    Chromatography in stable expanded beds enables proteins to be recovered directly from cultivations of microorganisms or cells and preparations of disrupted cells, without the need for prior removal of suspended solids. The general performance of an expanded bed is comparable to a packed bed owing to reduced mixing of the adsorbent particles in the column. However, optimal operating conditions are more restricted than in a packed bed due to the dependence of bed expansion on the size and density of the adsorbent particles as well as the viscosity and density of the feedstock. The feedstock composition may become the most limiting restriction owing to interactions of adsorbent particles with cell surfaces, DNA and other substances, leading to their aggregation and consequently to bed instabilities and channeling. Despite these difficulties, expanded-bed chromatography has found widespread applications in the large scale purification of proteins from mammalian cell and microbial feedstocks in industrial bioprocessing. The basics and implementation of expanded-bed chromatography, its advantages as well as problems encountered in the use of this technique for the direct extraction of proteins from unclarified feedstocks are addressed.

  1. Índice de adiposidad corporal como predictor de obesidad y de síndrome metabólico en adultos de Bogotá, Colombia

    OpenAIRE

    González-Ruíz, Katherine; Ramírez-Vélez, Robinson; Correa Bautista, Jorge Enrique

    2015-01-01

    Recientemente, Bergman et al. desarrollaron el índice de adiposidad corporal (IAC), como un marcador de obesidad por exceso de grasa corporal en la práctica clínica. En este estudio se evaluó la validez del IAC como marcador de obesidad por exceso de adiposidad, además de examinar la capacidad predictiva del IAC con componentes e índices metabólicos asociados al SM en adultos de Bogotá, Colombia.

  2. The analysis of aqueous mixtures using liquid chromatography-electrospray mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Johnson, Steven [Iowa State Univ., Ames, IA (United States)

    1999-02-12

    The focus of this dissertation is the use of chromatographic methods coupled with electrospray mass spectrometry (ES-MS) for the determination of both organic and inorganic compounds in aqueous solutions. The combination of liquid chromatography (LC) methods and ES-MS offers one of the foremost methods for determining compounds in complex aqueous solutions. In this work, LC-ES-MS methods are devised using ion exclusion chromatography, reversed phase chromatography, and ion exchange chromatography, as well as capillary electrophoresis (CE). For an aqueous sample, these LC-ES-MS and CE-ES-MS techniques require no sample preparation or analyte derivatization, which makes it possible to observe a wide variety of analytes as they exist in solution. The majority of this work focuses on the use of LC-ES-MS for the determination of unknown products and intermediates formed during electrochemical incineration (ECI), an experimental waste remediation process. This report contains a general introduction to the project and the general conclusions. Four chapters have been removed for separate processing. Titles are: Chapter 2: Determination of small carboxylic acids by ion exclusion chromatography with electrospray mass spectrometry; Chapter 3: Electrochemical incineration of benzoquinone in aqueous media using a quaternary metal oxide electrode in the absence of a soluble supporting electrolyte; Chapter 4: The determination of electrochemical incineration products of 4-chlorophenol by liquid chromatography-electrospray mass spectrometry; and Chapter 5: Determination of small carboxylic acids by capillary electrophoresis with electrospray mass spectrometry.

  3. Development and Implementation of a Quality Improvement Process for Echocardiographic Laboratory Accreditation.

    Science.gov (United States)

    Gilliland, Yvonne E; Lavie, Carl J; Ahmad, Homaa; Bernal, Jose A; Cash, Michael E; Dinshaw, Homeyar; Milani, Richard V; Shah, Sangeeta; Bienvenu, Lisa; White, Christopher J

    2016-03-01

    We describe our process for quality improvement (QI) for a 3-year accreditation cycle in echocardiography by the Intersocietal Accreditation Commission (IAC) for a large group practice. Echocardiographic laboratory accreditation by the IAC was introduced in 1996, which is not required but could impact reimbursement. To ensure high-quality patient care and community recognition as a facility committed to providing high-quality echocardiographic services, we applied for IAC accreditation in 2010. Currently, there is little published data regarding the IAC process to meet echocardiography standards. We describe our approach for developing a multicampus QI process for echocardiographic laboratory accreditation during the 3-year cycle of accreditation by the IAC. We developed a quarterly review assessing (1) the variability of the interpretations, (2) the quality of the examinations, (3) a correlation of echocardiographic studies with other imaging modalities, (4) the timely completion of reports, (5) procedure volume, (6) maintenance of Continuing Medical Education credits by faculty, and (7) meeting Appropriate Use Criteria. We developed and implemented a multicampus process for QI during the 3-year accreditation cycle by the IAC for Echocardiography. We documented both the process and the achievement of those metrics by the Echocardiography Laboratories at the Ochsner Medical Institutions. We found the QI process using IAC standards to be a continuous educational experience for our Echocardiography Laboratory physicians and staff. We offer our process as an example and guide for other echocardiography laboratories who wish to apply for such accreditation or reaccreditation. © 2016, Wiley Periodicals, Inc.

  4. Data model for the collaboration between land administration systems and agricultural land parcel identification systems.

    Science.gov (United States)

    Inan, Halil Ibrahim; Sagris, Valentina; Devos, Wim; Milenov, Pavel; van Oosterom, Peter; Zevenbergen, Jaap

    2010-12-01

    The Common Agricultural Policy (CAP) of the European Union (EU) has dramatically changed after 1992, and from then on the CAP focused on the management of direct income subsidies instead of production-based subsidies. For this focus, Member States (MS) are expected to establish Integrated Administration and Control System (IACS), including a Land Parcel Identification System (LPIS) as the spatial part of IACS. Different MS have chosen different solutions for their LPIS. Currently, some MS based their IACS/LPIS on data from their Land Administration Systems (LAS), and many others use purpose built special systems for their IACS/LPIS. The issue with these different IACS/LPIS is that they do not have standardized structures; rather, each represents a unique design in each MS, both in the case of LAS based or special systems. In this study, we aim at designing a core data model for those IACS/LPIS based on LAS. For this purpose, we make use of the ongoing standardization initiatives for LAS (Land Administration Domain Model: LADM) and IACS/LPIS (LPIS Core Model: LCM). The data model we propose in this study implies the collaboration between LADM and LCM and includes some extensions. Some basic issues with the collaboration model are discussed within this study: registration of farmers, land use rights and farming limitations, geometry/topology, temporal data management etc. For further explanation of the model structure, sample instance level diagrams illustrating some typical situations are also included. Copyright © 2010 Elsevier Ltd. All rights reserved.

  5. Safety operation of chromatography column system with discharging hydrogen radiolytically generated

    International Nuclear Information System (INIS)

    Watanabe, S; Sano, Y.; Nomura, K.; Koma, Y.; Okamoto, Y.

    2015-01-01

    The extraction chromatography technology is one of the promising methods for the partitioning of minor actinides (Am and Cm) from spent nuclear fuels. In the extraction chromatography system, the accumulation of hydrogen gas in the chromatography column is suspected to lead to fire or explosion. In order to prevent hazardous accidents, it is necessary to evaluate behaviors of gas radiolytically generated inside the column. In this study, behaviors of gas inside the extraction chromatography column were investigated through experiments and Computation Fluid Dynamics (CFD) simulation. N_2 gas once accumulated as bubbles in the packed bed was hardly discharged by the flow of mobile phase. However, the CFD simulation and X-ray imaging on γ-ray irradiated column revealed that during operation the hydrogen gas generated in the column was dissolved into the mobile phase without accumulation and then discharged. (authors)

  6. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  7. ANALYSIS AND IDENTIFICATION SPIKING CHEMICAL COMPOUNDS RELATED TO CHEMICAL WEAPON CONVENTION IN UNKNOWN WATER SAMPLES USING GAS CHROMATOGRAPHY AND GAS CHROMATOGRAPHY ELECTRON IONIZATION MASS SPECTROMETRY

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

    Full Text Available The identification and analysis of chemical warfare agents and their degradation products is one of important component for the implementation of the convention. Nowadays, the analytical method for determination chemical warfare agent and their degradation products has been developing and improving. In order to get the sufficient analytical data as recommended by OPCW especially in Proficiency Testing, the spiking chemical compounds related to Chemical Weapon Convention in unknown water sample were determined using two different techniques such as gas chromatography and gas chromatography electron-impact ionization mass spectrometry. Neutral organic extraction, pH 11 organic extraction, cation exchanged-methylation, triethylamine/methanol-silylation were performed to extract the chemical warfare agents from the sample, before analyzing with gas chromatography. The identification of chemical warfare agents was carried out by comparing the mass spectrum of chemicals with mass spectrum reference from the OPCW Central Analytical Database (OCAD library while the retention indices calculation obtained from gas chromatography analysis was used to get the confirmation and supported data of  the chemical warfare agents. Diisopropyl methylphosphonate, 2,2-diphenyl-2-hydroacetic acid and 3-quinuclidinol were found in unknown water sample. Those chemicals were classified in schedule 2 as precursor or reactant of chemical weapons compound in schedule list of Chemical Weapon Convention.   Keywords: gas chromatography, mass spectrometry, retention indices, OCAD library, chemical warfare agents

  8. Avaliação da aceitação de "chips" de mandioca Acceptance evaluation of cassava chips

    Directory of Open Access Journals (Sweden)

    Regina Kitagawa Grizotto

    2003-12-01

    Full Text Available Pré-tratamentos como o cozimento, a fermentação natural e a secagem parcial foram aplicados em raízes de mandioca, visando a obtenção de "chips" comestíveis. A avaliação sensorial foi feita com base na aceitação e aparência dos "chips" das variedades IAC Mantiqueira e IAC 576.70. Trinta consumidores potenciais do produto foram selecionados em função da disponibilidade e interesse em participar dos testes. Foi utilizada escala hedônica de 7 pontos, onde os provadores avaliaram as amostras delineadas em blocos casualizados. Os resultados obtidos mostraram que os "chips" controle e pré-cozidos foram aceitos sensorialmente, apresentado médias de 5,1 (gostei ligeiramente para IAC Mantiqueira e 6,0 (gostei moderadamente para IAC 576.70. Os "chips" pré-fermentados de ambas variedades foram rejeitados. Os termos de agrado mais comentados pelos provadores foram "sabor de mandioca", "crocância" e "textura". Os termos de desagrado mais citados incluem "textura dura", "falta sabor de mandioca" e "gosto de óleo". Os provadores consideraram adequada a aparência dos "chips" de ambas variedades, sendo ligeiramente preferida a aparência dos "chips" da IAC 576.70, com exceção dos "chips" cozidos por 8 minutos e os fermentados, rejeitados pelos consumidores. A cor amarela da polpa pode ter influenciado a aceitação da variedade IAC 576.70. A composição centesimal e o teor de fibras na mandioca in natura e, o teor de lipídeos em "chips" de mandioca, também foram apresentados.Pre-treatments such as cooking, natural fermentation and partial drying were applied to cassava roots, aimed at obtaining edible cassava chips. The sensory evaluation was based on the acceptance and appearance of the chips, using the varieties IAC Mantiqueira and IAC 576.70. Thirty potential consumers of the product were selected based on their availability and interest. A 7-point hedonic scale was used, all the judges evaluating all the samples using a randomised

  9. Preparative supercritical fluid chromatography: A powerful tool for chiral separations.

    Science.gov (United States)

    Speybrouck, David; Lipka, Emmanuelle

    2016-10-07

    In 2012, the 4 biggest pharmaceutical blockbusters were pure enantiomers and separating racemic mixtures is now frequently a key step in the development of a new drug. For a long time, preparative liquid chromatography was the technique of choice for the separation of chiral compounds either during the drug discovery process to get up to a hundred grams of a pure enantiomer or during the clinical trial phases needing kilograms of material. However the advent of supercritical Fluid Chromatography (SFC) in the 1990s has changed things. Indeed, the use of carbon dioxide as the mobile phase in SFC offers many advantages including high flow rate, short equilibration time as well as low solvent consumption. Despite some initial teething troubles, SFC is becoming the primary method for preparative chiral chromatography. This article will cover recent developments in preparative SFC for the separation of enantiomers, reviewing several aspects such as instrumentation, chiral stationary phases, mobile phases or purely preparative considerations including overloading, productivity or large scale chromatography. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Adaptation to high throughput batch chromatography enhances multivariate screening.

    Science.gov (United States)

    Barker, Gregory A; Calzada, Joseph; Herzer, Sibylle; Rieble, Siegfried

    2015-09-01

    High throughput process development offers unique approaches to explore complex process design spaces with relatively low material consumption. Batch chromatography is one technique that can be used to screen chromatographic conditions in a 96-well plate. Typical batch chromatography workflows examine variations in buffer conditions or comparison of multiple resins in a given process, as opposed to the assessment of protein loading conditions in combination with other factors. A modification to the batch chromatography paradigm is described here where experimental planning, programming, and a staggered loading approach increase the multivariate space that can be explored with a liquid handling system. The iterative batch chromatography (IBC) approach is described, which treats every well in a 96-well plate as an individual experiment, wherein protein loading conditions can be varied alongside other factors such as wash and elution buffer conditions. As all of these factors are explored in the same experiment, the interactions between them are characterized and the number of follow-up confirmatory experiments is reduced. This in turn improves statistical power and throughput. Two examples of the IBC method are shown and the impact of the load conditions are assessed in combination with the other factors explored. Copyright © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Narrow duplicated internal auditory canal: radiological findings and review of the literature

    International Nuclear Information System (INIS)

    Demir, Oezguen Ilhan; Cakmakci, Handan; Men, Sueleyman; Erdag, Taner Kemal

    2005-01-01

    Narrow duplicated internal auditory canal (IAC) is a rare malformation of the temporal bone that is associated with ipsilateral congenital sensorineural hearing loss. This may be an isolated finding or a part of a syndrome. Radiological examination should demonstrate aplasia or hypoplasia of the neural components of the narrow IAC, to guide the surgical approach. We report a 7-year-old boy with Klippel-Feil syndrome with a narrow double IAC with no sensorineural hearing loss but with conductive hearing loss. In this patient, the IAC consisted of two separate narrow bony canals clearly seen on 3D temporal bone CT and one nerve that was delineated on MRI. The contralateral external auditory canal was stenotic and the ossicles were dysplastic. (orig.)

  12. Environmental Quality Information Analysis Center multi-year plan

    International Nuclear Information System (INIS)

    Rivera, R.G.; Das, S.; Walsh, T.E.

    1992-09-01

    An information analysis center (IAC) is a federal resource that provides technical information for a specific technology field. An IAC links an expert technical staff with an experienced information specialist group, supported by in-house or external data bases to provide technical information and maintain a corporate knowledge in a technical area. An IAC promotes the rapid transfer of technology among its users and provides assistance in adopting new technology and predicting and assessing emerging technology. This document outlines the concept, requirements, and proposed development of an Environmental Quality IAC (EQIAC). An EQIAC network is composed of several nodes, each of which has specific technology capabilities. This document outlines strategic and operational objectives for the phased development of one such node of an EQIAC network

  13. Lowland rice yield estimates based on air temperature and solar radiation

    International Nuclear Information System (INIS)

    Pedro Júnior, M.J.; Sentelhas, P.C.; Moraes, A.V.C.; Villela, O.V.

    1995-01-01

    Two regression equations were developed to estimate lowland rice yield as a function of air temperature and incoming solar radiation, during the crop yield production period in Pindamonhangaba, SP, Brazil. The following rice cultivars were used: IAC-242, IAC-100, IAC-101 and IAC-102. The value of optimum air temperature obtained was 25.0°C and of optimum global solar radiation was 475 cal.cm -2 , day -1 . The best agrometeorological model was the one that related least deviation of air temperature and solar radiation in relation to the optimum value obtained through a multiple linear regression. The yield values estimated by the model showed good fit to actual yields of lowland rice (less than 10%). (author) [pt

  14. Final Technical Report

    Energy Technology Data Exchange (ETDEWEB)

    Bohdan W. Oppenheim; Rudolf Marloth

    2007-10-26

    Executive Summary The document contains Final Technical Report on the Industrial Assessment Center Program at Loyola Marymount University in Los Angeles, covering the contract period of 9/1/2002 to 11/30/2006, under the contract DE-FC36-02GO 12073. The Report describes six required program tasks, as follows: TASK 1 is a summary of the assessments performed over the life of the award: 77 assessments were performed, 595 AR were recommended, covering a very broad range of manufacturing plants. TASK 2 is a description of the efforts to promote and increase the adoption of assessment recommendations and employ innovative methods to assist in accomplishing these goals. The LMU IAC has been very successful in accomplishing the program goals, including implemented savings of $5,141,895 in energy, $10,045,411 in productivity and $30,719 in waste, for a total of $15,218,025. This represents 44% of the recommended savings of $34,896,392. TASK 3 is a description of the efforts promoting the IAC Program and enhancing recruitment efforts for new clients and expanded geographic coverage. LMU IAC has been very successful recruiting new clients covering Southern California. Every year, the intended number of clients was recruited. TASK 4 describes the educational opportunities, training, and other related activities for IAC students. A total of 38 students graduated from the program, including 2-3 graduate students every semester, and the remainder undergraduate students, mostly from the Mechanical Engineering Department. The students received formal weekly training in energy (75%) and productivity (25). All students underwent extensive safety training. All students praised the IAC experience very highly. TASK 5 describes the coordination and integration of the Center activities with other Center and IAC Program activities, and DOE programs. LMU IAC worked closely with MIT, and SDSU IAC and SFSU IAC, and enthusiastically supported the SEN activities. TASK 6 describes other tasks

  15. Variability of tracer transport in spring/summer Arctic stratosphere simulated by CESM-WACCM

    Science.gov (United States)

    Thiéblemont, Rémi; Matthes, Katja; Hansen, Felicitas; Huret, Nathalie

    2014-05-01

    Recent observational and modeling transport studies of Arctic stratospheric final warmings have shown that tropical/subtropical air can be transported to high latitudes and remain confined within a long-lived "frozen-in" anticyclone (FrIAC), embedded in the summer easterlies for several months. A climatology of these sporadic events has shown that their frequency of occurrence considerably increased over the last decade: among the nine cases detected over the period 1960-2011, five occurred between 2002 and 2011.Although a stratospheric favorable preconditioning for their occurrence were identified, the causes of such an increase are not yet understood. In this study, a chemistry climate model is used for the first time to investigate FrIACs characteristics and variability. Simulations were performed with the NCAR's Community Earth System Model (CESM), a coupled model system including an interactive ocean (POP2), land (CLM4), sea ice (CICE), and atmosphere (NCAR's Whole Atmosphere Community Climate Model (WACCM)). To detect low-latitude air masses characterizing FrIACs, daily 3-D output of temperature, horizontal wind and pressure are used to calculate the potential vorticity equivalent latitude (PVEL) distribution onto various isentropic levels in the range 700 K - 1200 K. Additionally, anticyclones are identified by using an algorithm designed to detect systematically vortex edges. To classify an event as a FrIAC, we require that the intrusion contains air masses from low-latitudes (below PVEL=40°N), reaches the polar region (beyond 60°N), and is collocated with an anticyclonic eddy. Among the 145 years analyzed (1955-2099), from a simulation with natural forcing conditions only, 20 FrIACs are found. They occur predominantly under a strong and abrupt winter-to-summer dynamical transitions which are driven by large planetary wave activity. FrIACs characteristics (i.e. spatial extent and duration), are overall consistent by comparing with FrIACs detected in ERA

  16. Determinação dos índices de cristalinidade de fibras celulósicas Crystallinity index determination on cellulosic fibers

    Directory of Open Access Journals (Sweden)

    Rose Marry Araújo Gondim Tomaz

    1994-01-01

    Full Text Available No presente estudo, foi avaliada a introdução de métodos de análises de micro-estrutura de fibras celulósicas. O algodão utilizado, proveniente das variedades IAC 17, IAC 19 e IAC 20, foi colhido em dez localidades do ensaio regional de variedades do Estado de São Paulo, no ano agrícola de 1985/86. Amostras de fibras de viscose, rami e rami tratado quimicamente com ácido clorídrico, também foram usadas, a fim de estabelecer uma relação entre os dois sistemas de determinação dos índices de cristalinidade. Utilizaram-se os métodos empíricos de difratometria de raios X e espectroscopia de infravermelho para as determinações dos índices de cristalinidade: o obtido por espectroscopia de infravermelho permitiu a diferenciação de variedades de algodoeiro IAC, enquanto o proposto por difratometria de raios X não possibilitou essa diferença. As propriedades físicas das fibras de variedades de algodoeiro IAC não se correlacionaram com os índices de cristalinidade obtidos nos dois processos. Os métodos usados para a determinação de tais índices foram altamente correlacionados (r = 0,95, empregando-se amostras de celulose com tratamento diferenciado.The purpose of this work was to develop analytical techniques for structural characterization of cellulosic fibers. To establish a relationship between the two methods that determine crystallinity index, three varieties of cotton (IAC 17, IAC 19, and IAC 20 and fibers of viscose, rami and rami chemical treated were used. Two empirical methods, x-ray diffraction and infrared spectroscopy, were used to evaluate the crystallinity index. Differentiation of IAC cotton varieties was possible with the crystallinity index obtained by infrared spectroscopy; but, not with the x-ray diffraction method. The crystallinity index obtained by these two methods had no correlation with physical properties of cotton fibers. When cellulose fibers with different treatment were assayed, there was a

  17. Acid dissociation constant and apparent nucleophilicity of lysine-501 of the alpha-polypeptide of sodium and potassium ion activated adenosinetriphosphatase

    International Nuclear Information System (INIS)

    Xu, K.Y.

    1989-01-01

    A combination of competitive labeling with [ 3 H]acetic anhydride and immunoaffinity chromatography is described that permits the assignment of the acid dissociation constant and the absolute nucleophilicity of individual lysines in a native enzyme. The acid dissociation constant of lysine-501 of the alpha-polypeptide in native (Na+ + K+)-ATPase was determined. This lysine had a normal pKa of 10.4. The rate constant for the reaction of the free base of lysine-501 with acetic anhydride at 10 degrees C is 400 M-1 s-1. This value is only 30% that for a fully accessible lysine in a protein. The lower than normal apparent nucleophilicity suggests that lysine-501 is hindered from reacting with its intrinsic nucleophilicity by the tertiary structure of the enzyme and is consistent with its location within a pocket that forms the active site upon the surface of the native protein

  18. Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

    NARCIS (Netherlands)

    Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

    Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an

  19. VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis. Program. Summary of reports

    International Nuclear Information System (INIS)

    2001-01-01

    Program and summary of reports of the VIII All-Russian symposium on molecular liquid chromatography and capillary electrophoresis are performed. The meeting took place 15-19 October, 2001 in Moscow. Many problems of liquid and ion exchange chromatography, capillary electrophoresis, thin-layer chromatography have been discussed extensively. Reports covering properties of sorbents and devices for chromatography are incorporated in the collection [ru

  20. Purification of radiolabeled RNA using sephadex G-15 or G-50 chromatography

    International Nuclear Information System (INIS)

    Yoo, Beong Gyu; Lee, Jong Seok

    1998-01-01

    We attempted to purify radiolabeled RNA using Sephadex G-15 and G-50 chromatography instead of commercial RNA purification kit. In the Sephadex G-15 chromatography the major portion of RNA was eluted in the fractions ranging from 3rd to 5th whereas broad elution profile of RNA was obtained from the Sephadex G-50 chromatography. The elution profile and purity of RNA obtained from Sephadex G-15 chromatography was very similar to that by commercial RNA purification kit. Furthermore, operating time required for purification of RNA by Sephadex G-15 was rather smaller than that by commercial kit. Overall results suggest that the purification of radiolabeled RNA using Sephadex G-15 is more money and time saving than using commercial RNA purification kit

  1. Gradient High Performance Liquid Chromatography Method ...

    African Journals Online (AJOL)

    Purpose: To develop a gradient high performance liquid chromatography (HPLC) method for the simultaneous determination of phenylephrine (PHE) and ibuprofen (IBU) in solid ..... nimesulide, phenylephrine. Hydrochloride, chlorpheniramine maleate and caffeine anhydrous in pharmaceutical dosage form. Acta Pol.

  2. Carbon nanoparticles from corn stalk soot and its novel application as stationary phase of hydrophilic interaction chromatography and per aqueous liquid chromatography

    International Nuclear Information System (INIS)

    Li Yuanyuan; Xu Luan; Chen Tong; Liu Xiaoyan; Xu Zhigang; Zhang Haixia

    2012-01-01

    Highlights: ► Carbon nanoparticles (6–18 nm in size) were prepared from corn stalk soot. ► CNPs-based silica were used as novel chromatography stationary phase. ► The new phase shows good separation selectivity for polar compounds. ► The new phase had the similar retention for polar probes in HILIC and PALC modes. ► In contrast to PALC, under HILIC conditions high efficiencies were achieved. - Abstract: Carbon nanoparticles (CNPs) (6–18 nm in size) were prepared by refluxing corn stalk soot in nitric acid. The obtained acid-oxidized CNPs are soluble in water due to the existence of carboxylic and hydroxyl groups. 13 C NMR measurement shows the CNPs are mainly of sp 2 and sp 3 carbon structure different from CNPs obtained from candle soot and natural gas soot. Furthermore, these CNPs exhibit unique photoluminescence properties. Interestingly, the CNPs might be exploited to immobilize on the surface of porous silica particles as chromatographic stationary phase. The resultant packing material was evaluated by high-performance liquid chromatography, indicating that the new stationary phase could be used in hydrophilic interaction liquid chromatography (HILIC) and per aqueous liquid chromatography (PALC) modes. The separation of five nucleosides, four sulfa compounds and safflower injection was achieved by using the new column in the HILIC and PALC modes, respectively.

  3. Trends in the analysis of natural gas by capillary gas chromatography

    NARCIS (Netherlands)

    Cramers, C.A.M.G.; Rossum, van G.J.

    1986-01-01

    The importance of correct determination of physical and chemical properties of natural gas is evident. The calculation of calorific value or hydrocarbon dew point requires detailed analysis as can be provided by gas chromatography. Analysis by gas chromatography is a necessary complement to direct

  4. Hyphenated and comprehensive liquid chromatography × gas chromatography-mass spectrometry for the identification of Mycobacterium tuberculosis.

    Science.gov (United States)

    Mourão, Marta P B; Denekamp, Ilse; Kuijper, Sjoukje; Kolk, Arend H J; Janssen, Hans-Gerd

    2016-03-25

    Tuberculosis is one of the world's most emerging public health problems, particularly in developing countries. Chromatography based methods have been used to tackle this epidemic by focusing on biomarker detection. Unfortunately, interferences from lipids in the sputum matrix, particularly cholesterol, adversely affect the identification and detection of the marker compounds. The present contribution describes the serial combination of normal phase liquid chromatography (NPLC) with thermally assisted hydrolysis and methylation followed by gas chromatography-mass spectrometry (THM-GC-MS) to overcome the difficulties of biomarker evaluation. The in-series combination consists of an LC analysis where fractions are collected and then transferred to the THM-GC-MS system. This was either done with comprehensive coupling, transferring all the fractions, or with hyphenated interfacing, i.e. off-line multi heart-cutting, transferring only selected fractions. Owing to the high sensitivity and selectivity of LC as a sample pre-treatment method, and to the high specificity of the MS as a detector, this analytical approach, NPLC × THM-GC-MS, is extremely sensitive. The results obtained indicate that this analytical set-up is able to detect down to 1 × 10(3) mycobacteria/mL of Mycobacterium tuberculosis strain 124, spiked in blank sputum samples. It is a powerful analytical tool and also has great potential for full automation. If further studies demonstrate its usefulness when applied blind in real sputum specimens, this technique could compete with the current smear microscopy in the early diagnosis of tuberculosis. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Affinity chromatography: A versatile technique for antibody purification.

    Science.gov (United States)

    Arora, Sushrut; Saxena, Vikas; Ayyar, B Vijayalakshmi

    2017-03-01

    Antibodies continue to be extremely utilized entities in myriad applications including basic research, imaging, targeted delivery, chromatography, diagnostics, and therapeutics. At production stage, antibodies are generally present in complex matrices and most of their intended applications necessitate purification. Antibody purification has always been a major bottleneck in downstream processing of antibodies, due to the need of high quality products and associated high costs. Over the years, extensive research has focused on finding better purification methodologies to overcome this holdup. Among a plethora of different techniques, affinity chromatography is one of the most selective, rapid and easy method for antibody purification. This review aims to provide a detailed overview on affinity chromatography and the components involved in purification. An array of support matrices along with various classes of affinity ligands detailing their underlying working principles, together with the advantages and limitations of each system in purifying different types of antibodies, accompanying recent developments and important practical methodological considerations to optimize purification procedure are discussed. Copyright © 2016 Elsevier Inc. All rights reserved.

  6. [Analysis of microalbuminuria with immunonephelometry and high performance liquid chromatography. Evaluation of new criteria].

    Science.gov (United States)

    Markó, Lajos; Molnár, Gergo Attila; Wagner, Zoltán; Koszegi, Tamás; Matus, Zoltán; Mohás, Márton; Kuzma, Mónika; Szijártó, István András; Wittmann, István

    2008-01-13

    Hypertension as well as type 2 diabetes mellitus is a major factor in population mortality. Both diseases damage the endothelium, the early sign of which is microalbuminuria, which can be screened by dipstick and can be diagnosed by using immuno-based and high performance liquid chromatography methods. Using high performance liquid chromatography, the non-immunoreactive albumin can be detected as well. The authors aimed at the examination of albuminuria in the case of immunonephelometrically negative patients with high performance liquid chromatography, in diabetic and hypertensive and non-diabetic hypertensive populations. The authors also wanted to compare the present (albumin-creatinine ratio: male: > or =2.5 mg/mmol, female: > or =3.5 mg/mmol) and a new criteria of the Heart Outcomes Prevention Evaluation study (patients without diabetes: immunological method, > or =0.7 mg/mmol; high performance liquid chromatography, > or =3.1 mg/mmol; individuals with diabetes: immunological method, > or =1.4 mg/mmol; high performance liquid chromatography, > or =5.2 mg/mmol) of microalbuminuria. Examination of fresh urines of 469 microalbuminuria negative patients by dipstick were performed by immunonephelometry. Patients, who were microalbuminuria negative by immunonephelometry as well, were further analyzed by high performance liquid chromatography using the Accumintrade mark Kit, based on size-exclusion chromatography. Three times higher albuminuria were found with high performance liquid chromatography than with immunonephelometry. The intraindividual coefficient of variation did not differ in the two methods (37 +/- 31% vs. 40 +/- 31%, p = 0.869; immunonephelometry vs. high performance liquid chromatography; mean +/- standard deviation). Using the present criteria for microalbuminuria, 43% of immunonephelometrically negative patients proved to be microalbuminuric by high performance liquid chromatography. Using the new criteria of the Heart Outcomes Prevention

  7. Characterization of heat tolerance in wheat cultivars and effects on production components

    Directory of Open Access Journals (Sweden)

    Adérico Júnior Badaró Pimentel

    2015-04-01

    Full Text Available Abstract: There is a need for heat tolerant wheat cultivars adapted to the expansion of cultivation areas in warmer regions due to the high demand of this cereal for human consumption. The objective of this study was to evaluate the effect of high temperatures on grain yield and yield components of wheat and characterize heat tolerant wheat genotypes at different development stages. The genotypes were evaluated in the field with and without heat stress. High temperatures reduced the number of spikelets per spike (21%, number of grains per spike (39%, number of grains per spikelet (23%, 1000-grain weight (27% and grain yield (79%. Cultivars MGS 1 Aliança, Embrapa 42, IAC 24-Tucuruí and IAC 364-Tucuruí III are the most tolerant to heat stress between the stages double ridge and terminal spikelet; MGS 1 Aliança, BRS 264, IAC 24-Tucuruí, IAC 364-Tucuruí III and VI 98053, between meiosis and anthesis; and BRS 254, IAC-24-Tucuruí, IAC-364-Tucuruí III and VI 98053, between anthesis and physiological maturity. High temperatures reduce grain yield and yield components. The number of grains per spike is the most reduced component under heat stress. The genotypes differed in tolerance to heat stress in different developmental stages.

  8. Gamma radiation effects at color, antioxidant capacity and fatty acid profile in peanut (Arachis hypogaea L.); Efeitos da radiacao gama na cor, capacidade antioxidante e perfil de acidos graxos em amendoim (Arachis hypogaea L.)

    Energy Technology Data Exchange (ETDEWEB)

    Camargo, Adriano Costa de; Canniatti-Brazaca, Solange Guidolin; Mansi, Debora Niero; Domingues, Maria Antonia Calori [Escola Superior de Agricultura Luiz de Queiroz (ESALQ/USP), Piracicaba, SP (Brazil). Dept. de Agroindustria, Alimentos e Nutricao; Arthur, Valter, E-mail: arthur@cena.usp.b [Centro de Energia Nuclear na Agricultura (CENA/USP), Piracicaba, SP (Brazil)

    2011-01-15

    Irradiation is efficient at extinction fungi contamination in peanuts. Peanuts have high biologic value protein, minerals, vitamin E, complex B, and high concentration of lipids. The objective of this research is to evaluate the gamma irradiation effect on color, total phenolic, antioxidant activity, and fatty acid profile in peanuts (Arachis hypogaea L.). Cultivars IAC-Tatu ST and IAC-Runner 886 were submitted to gamma radiation with doses of 5.0; 7.5; 10.0, and 15.0 kGy and storage at room temperature. There was no significant difference in the color of IAC-Tatu ST. However, significant difference was found in the luminosity and Chroma in IAC-Runner 886. Total fenolics differed from the control with 33.27 mg.g{sup -1} and treatment dose of 10.0 kGy with 58.60 mg.g{sup -1} in IAC-Tatu ST. This parameter not had significant difference in IAC-Runner 886 and the control with 51.59 mg.g{sup -1}. The antioxidant activity did not present significant difference with a dose of 10.0 kGy, recommended for the elimination of fungi in peanuts. The dose of 10.0 kGy showed a decrease in saturated fatty acids, increase in unsaturated fatty acids, and an increase in linolleic acid. The oleic/linoleic relation decreased justifying further research correlating storage and oxidative stability. (author)

  9. The investigation of copper-based impregnated activated carbons prepared from water-soluble materials for broad spectrum respirator applications

    Energy Technology Data Exchange (ETDEWEB)

    Smith, J.W.H.; Westreich, P.; Abdellatif, H.; Filbee-Dexter, P.; Smith, A.J. [Department of Physics and Atmospheric Science, Dalhousie University, Halifax, Nova Scotia, B3H 3J5 (Canada); Wood, T.E. [3M Company, St. Paul, MN, 55144 (United States); Croll, L.M.; Reynolds, J.H. [3M Canada Company, Brockville, Ontario, K6V 5V8 (Canada); Dahn, J.R., E-mail: jeff.dahn@dal.ca [Department of Physics and Atmospheric Science, Dalhousie University, Halifax, Nova Scotia, B3H 3J5 (Canada); Department of Chemistry, Dalhousie University, Halifax, Nova Scotia, B3H 4J3 (Canada)

    2010-08-15

    The preparation of impregnated activated carbons (IACs) from aqueous, copper-containing solutions for broad spectrum gas filtration applications is studied here. Several samples were studied to determine the effect that impregnant loading, impregnant distribution and impregnant recipe had on the overall performance. Dynamic flow testing was used to determine the gas filtration capacity of the IAC samples versus a variety of challenge gases. X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) were used to characterize the impregnant distribution on the carbon as a function of impregnant loading. Oven tests were performed to determine the thermal stability of the IAC samples exposed to elevated temperatures. The role impregnant distribution plays in gas filtration capacity and the overall performance of the IAC samples is discussed. The IAC samples prepared in this work were found to have gas filtration capacities as good as or better than broad spectrum respirator carbon samples prepared from the patent literature. IACs impregnated with an aqueous 2.4 M Cu(NO{sub 3}){sub 2}/0.04 M H{sub 3}PO{sub 4}.12MoO{sub 3}/4 M HNO{sub 3} solution that were heated to 200 deg. C under argon were found to have the best overall performance of the samples studied in this work.

  10. Simultaneous determination of niacin and pyridoxine at trace levels by using diode array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry.

    Science.gov (United States)

    Sel, Sabriye; Öztürk Er, Elif; Bakırdere, Sezgin

    2017-12-01

    A highly sensitive and simple diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method was developed for the simultaneous determination of niacin and pyridoxine in pharmaceutical drugs, tap water, and wastewater samples. To determine the in vivo behavior of niacin and pyridoxine, analytes were subjected to simulated gastric conditions. The calibration plots of the diode-array high-performance liquid chromatography and liquid chromatography with quadrupole time-of-flight tandem mass spectrometry method showed good linearity over a wide concentration range with close to 1.0 correlation coefficients for both analytes. The limit of detection/limit of quantitation values for liquid chromatography quadrupole time-of-flight tandem mass spectrometry analysis were 1.98/6.59 and 1.3/4.4 μg/L for niacin and pyridoxine, respectively, while limit of detection/limit of quantitation values for niacin and pyridoxine in high-performance liquid chromatography analysis were 3.7/12.3 and 5.7/18.9 μg/L, respectively. Recovery studies were also performed to show the applicability of the developed methods, and percentage recovery values were found to be 90-105% in tap water and 94-97% in wastewater for both analytes. The method was also successfully applied for the qualitative and quantitative determination of niacin and pyridoxine in drug samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Surface modification of chromatography adsorbents by low temperature low pressure plasma

    DEFF Research Database (Denmark)

    Arpanaei, Ayyoob; Winther-Jensen, Bjørn; Theodosiou, E.

    2010-01-01

    In this study we show how low temperature glow discharge plasma can be used to prepare bi-layered chromatography adsorbents with non-adsorptive exteriors. The commercial strong anion exchange expanded bed chromatography matrix, Q HyperZ, was treated with plasmas in one of two general ways. Using ...

  12. Hierarchical CaCO3 chromatography: a stationary phase based on biominerals.

    Science.gov (United States)

    Sato, Kosuke; Oaki, Yuya; Takahashi, Daisuke; Toshima, Kazunobu; Imai, Hiroaki

    2015-03-23

    In biomineralization, acidic macromolecules play important roles for the growth control of crystals through a specific interaction. Inspired by this interaction, we report on an application of the hierarchical structures in CaCO3 biominerals to a stationary phase of chromatography. The separation and purification of acidic small organic molecules are achieved by thin-layer chromatography and flash chromatography using the powder of biominerals as the stationary phase. The unit nanocrystals and their oriented assembly, the hierarchical structure, are suitable for the adsorption site of the target organic molecules and the flow path of the elution solvents, respectively. The separation mode is ascribed to the specific adsorption of the acidic molecules on the crystal face and the coordination of the functional groups to the calcium ions. The results imply that a new family of stationary phase of chromatography can be developed by the fine tuning of hierarchical structures in CaCO3 materials. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Bacterial Cell Wall Precursor Phosphatase Assays Using Thin-layer Chromatography (TLC) and High Pressure Liquid Chromatography (HPLC).

    Science.gov (United States)

    Pazos, Manuel; Otten, Christian; Vollmer, Waldemar

    2018-03-20

    Peptidoglycan encases the bacterial cytoplasmic membrane to protect the cell from lysis due to the turgor. The final steps of peptidoglycan synthesis require a membrane-anchored substrate called lipid II, in which the peptidoglycan subunit is linked to the carrier lipid undecaprenol via a pyrophosphate moiety. Lipid II is the target of glycopeptide antibiotics and several antimicrobial peptides, and is degraded by 'attacking' enzymes involved in bacterial competition to induce lysis. Here we describe two protocols using thin-layer chromatography (TLC) and high pressure liquid chromatography (HPLC), respectively, to assay the digestion of lipid II by phosphatases such as Colicin M or the LXG toxin protein TelC from Streptococcus intermedius . The TLC method can also monitor the digestion of undecaprenyl (pyro)phosphate, whereas the HPLC method allows to separate the di-, mono- or unphosphorylated disaccharide pentapeptide products of lipid II.

  14. Índice de adiposidad corporal como predictor de obesidad y de síndrome metabólico en adultos de Bogotá, Colombia

    OpenAIRE

    González-Ruíz, Katherine; Ramírez-Vélez, Robinson; Correa Bautista, Jorge Enrique

    2015-01-01

    Recientemente, Bergman et al. desarrollaron el índice de adiposidad corporal (IAC), como un marcador de obesidad por exceso de grasa corporal en la práctica clínica. En este estudio se evaluó la validez del IAC como marcador de obesidad por exceso de adiposidad, además de examinar la capacidad predictiva del IAC con componentes e índices metabólicos asociados al SM en adultos de Bogotá, Colombia. Convocatoria FODEIN-USTA 2014 Nº 2013004

  15. Tillering of two wheat genotypes as affected by phosphorus levels=Perfilhamento de dois genótipos de trigo em função de doses de fósforo

    Directory of Open Access Journals (Sweden)

    Leonardo Theodoro Büll

    2012-07-01

    Full Text Available Tillering plays an important role in wheat yield potential and it is affected by genotype and environmental conditions. This work aimed to study the effects of phosphorus levels on tiller emergence, survival and contribution to yield potential of two wheat cultivars. The experiment was carried out under greenhouse conditions in Botucatu, São Paulo State, Brazil. A 2 x 5 factorial randomized block design with four replications was applied. Two wheat cultivars (IAC 370 and IAC 375 and five phosphorus levels (0, 150, 300, 450 and 600 mg dm-3 were evaluated in pots with 10 dm3 of a clayey Oxisol. Higher P levels increased tiller emergence, survival and yield, especially for secondary tillers. Tiller abortion levels were higher in IAC 370 cultivar whereas retention of formed tillers was higher in IAC 375. A participação de perfilhos na produção de grãos é de grande importância para a cultura do trigo, sendo influenciável pelas características do genótipo e condições do ambiente. O presente trabalho teve o objetivo de estudar o efeito de doses de fósforo (P na emissão, sobrevivência e contribuição produtiva de perfilhos de duas cultivares de trigo. O experimento foi conduzido em casa de vegetação em Botucatu, Estado de São Paulo. Foi adotado um esquema fatorial 2 x 5 em blocos casualizados com quatro repetições, sendo avaliadas duas cultivares de trigo (IAC 370 e IAC 375 e cinco doses de P (0, 150, 300, 450 e 600 mg dm-3. Quanto maior a dose de P, maior a emissão, a sobrevivência e a participação de perfilhos na produ��ão total de grãos, em especial para perfilhos secundários. A cultivar IAC 370 apresentou altas taxas de abortamento de perfilhos, enquanto a IAC 375 manteve grande parte dos perfilhos emitidos.

  16. 75 FR 9103 - Approval and Promulgation of Air Quality Implementation Plans; Illinois; NOX

    Science.gov (United States)

    2010-03-01

    ... recommend that you telephone John Summerhays, Environmental Scientist, at (312) 886-6067, before visiting... 35 IAC 217 Subpart W. Illinois' revision would add 35 IAC 217.751, the full text of which is: The...

  17. Purification of a 166mHo solution by successive high-performance liquid chromatography and gravitational chromatography for half-life determination

    International Nuclear Information System (INIS)

    Florence Gueguen; Helene Isnard; Carole Bresson; Celine Caussignac; Guillaume Stadelmann; Anthony Nonell; Sebastien Mialle; Karsten Kossert; Frederic Chartier

    2014-01-01

    A methodology to purify a 166m Ho solution has been developed by a combination of activity and mass concentration measurements in order to further determine the 166m Ho half-life. The isobaric interference at m/q ≃ 166 requires Ho purification from non-natural Er with a high purification degree due to the large amount of Ho as opposed to Er. The Ho/Er separation was achieved using high-performance liquid chromatography on a semi-preparative column followed by purification on gravitational chromatography. The efficiency of the separation was evaluated after precise determination of the Er isotopic composition. The purification methodology enabled to separate Ho from Er. (author)

  18. Arquitetura e dimensão do sistema radicular de sete porta-enxertos de videira no Norte do Estado do Paraná

    Directory of Open Access Journals (Sweden)

    Bordin Ivan

    2003-01-01

    Full Text Available Foi estudada a estrutura do sistema radicular de sete porta-enxertos de videira das cultivares IAC 572, Kobber 5BB, Rupestris du Lot, IAC 313, IAC 766, Ripária do Traviú e 420 A, com cinco anos de idade. As raízes foram expostas por escavação e avaliadas pelo programa SIARCS 3.0. Foi utilizado um diagrama de arquitetura radicular, atribuindo-se notas à conformação do sistema radicular. O 'IAC 572' apresentou a maior extensão de raízes e o '420 A', a menor. Os porta-enxertos não apresentaram diferença quanto à arquitetura do sistema radicular. Os mais vigorosos apresentaram maior proporção de raízes enoveladas.

  19. Industrial Assessment Center Program Impact Evaluation

    Energy Technology Data Exchange (ETDEWEB)

    Martin, M.A.

    2000-01-26

    This report presents the results of an evaluation of the U.S. Department of Energy's Industrial Assessment Center (IAC) Program. The purpose of this program is to conduct energy, waste, and productivity assessments for small to medium-sized industrial firms. Assessments are conducted by 30 university-based industrial assessment centers. The purpose of this project was to evaluate energy and cost savings attributable to the assessments, the trained alumni, and the Websites sponsored by this program. How IAC assessments, alumni, and Web-based information may influence industrial energy efficiency decision making was also studied. It is concluded that appreciable energy and cost savings may be attributed to the IAC Program and that the IAC Program has resulted in more active and improved energy-efficiency decision making by industrial firms.

  20. Impact of comprehensive two-dimensional gas chromatography with mass spectrometry on food analysis.

    Science.gov (United States)

    Tranchida, Peter Q; Purcaro, Giorgia; Maimone, Mariarosa; Mondello, Luigi

    2016-01-01

    Comprehensive two-dimensional gas chromatography with mass spectrometry has been on the separation-science scene for about 15 years. This three-dimensional method has made a great positive impact on various fields of research, and among these that related to food analysis is certainly at the forefront. The present critical review is based on the use of comprehensive two-dimensional gas chromatography with mass spectrometry in the untargeted (general qualitative profiling and fingerprinting) and targeted analysis of food volatiles; attention is focused not only on its potential in such applications, but also on how recent advances in comprehensive two-dimensional gas chromatography with mass spectrometry will potentially be important for food analysis. Additionally, emphasis is devoted to the many instances in which straightforward gas chromatography with mass spectrometry is a sufficiently-powerful analytical tool. Finally, possible future scenarios in the comprehensive two-dimensional gas chromatography with mass spectrometry food analysis field are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Supercritical fluid chromatography approach for a sustainable manufacture of new stereoisomeric anticancer agent.

    Science.gov (United States)

    Ghinet, Alina; Zehani, Yasmine; Lipka, Emmanuelle

    2017-10-25

    Two routes aimed at the manufacture of unprecedented stereoisomeric combretastatin A-4 analogue were described: flash chromatography vs supercritical fluid chromatography. The latter has many advantages over liquid chromatography and was therefore chosen for the small scale separation of methyl 1-[(3-hydroxy-4-methoxyphenyl) (3,4,5-trimethoxyphenyl)methyl]-5-oxo-l-prolinate 5, with potential antitumoral activity. After a screening of six different polysaccharide based chiral stationary phases and four co-solvents, the percentage of co-solvent, the flow-rate and the outlet pressure were optimized through a design of experiments (DoE). The preparation of 50mg of each stereoisomer was achieved successfully on a Chiralpak AD-H with isopropanol as a co-solvent. Productivity (kkd), solvent usage and environmental factor (E Factor) were calculated. Flash chromatography and supercritical fluid chromatography approaches were compared in terms of yield and purity of each stereoisomer manufactured. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Liquid chromatography in migration studies

    International Nuclear Information System (INIS)

    Carlsen, L.; Batsberg, W.

    1982-01-01

    Liquid chromatography ahs been suggested as a facile experimental technique to determine important physico-chemical properties, as permeability, porosity, dispersion-, diffusion-, and sorption charcteristics for geological material as chalk samples. The feasibility of the trechnique as a rapid method to evaluate the possible influence of changes in ground water composition on the migration behavior of radionuclides has been demonstrated

  3. Undergraduate Separations Utilizing Flash Chromatography

    Science.gov (United States)

    Horowitz, G.

    2000-02-01

    This article describes the procedures used to carry out four flash chromatography experiments: the isolation of the carotenes, chlorophylls and xanthophylls from a spinach extract; the separation of ß-carotene from tetraphenyl cyclopentadienone; the isolation of (+) and (-) carvone from caraway and spearmint oil; and the purification of benzil from benzoin. Apparatus used is nonbreakable, easy to use, and inexpensive.

  4. Qualidade da semente e senescência de genótipos de soja sob dois níveis de infestação de percevejos (Pentatomidae Quality of seeds and senescence of soybean genotypes under two levels of bugs infestation (Pentatomidae

    Directory of Open Access Journals (Sweden)

    Paulo Rogério Lustosa

    1999-08-01

    Full Text Available Este trabalho objetivou estudar a resistência de duas linhagens de soja, do programa de melhoramento do sabor da Universidade Federal de Viçosa, MG, cultivadas sob dois níveis de infestação de percevejos, em comparação com três cultivares de soja. Os genótipos estudados foram: CR-1, CR-3, Cristalina (linhagem paterna, Davis (padrão de suscetibilidade e IAC-100 (padrão de resistência. CR-1, CR-3, Davis e Cristalina, sob baixa infestação, produziram porcentagens de sementes normais semelhantes entre si (57%, e inferiores às de IAC-100 (77%. Sob alta infestação, CR-1, CR-3 e Cristalina produziram percentagens de sementes normais semelhantes entre si (22% e inferiores às de Davis (43% e IAC-100 (59%. Todos os genótipos apresentaram baixo grau de retenção foliar (menos que 6% quando cultivados sob baixa infestação, mas sob alta infestação, a CR-1 e IAC-100 apresentaram menores porcentagens de retenção foliar (menos que 5%, seguida por Davis e CR-3 (6-20% e Cristalina (21-40%. CR-1, IAC-100 e Davis não apresentaram plantas com caule verde sob baixa infestação, ao contrário do que foi registrado com CR-3 (3,6% e Cristalina (11%. IAC-100, CR-1 e Davis apresentaram menores porcentagens de plantas com caule verde (6,4, 10,3 e 18,3%, respectivamente que CR-3 (64,8% e Cristalina (77,3%.The objective of this research was to evaluate the genotypes CR-1 and CR-3, from the genetic improvement program of soybean flavor of the Federal University of Viçosa, in Viçosa, MG, Brazil, under two levels of Heteroptera infestation. The genotypes tested were CR-1, CR-3, Cristalina, Davis (susceptible genotype and IAC-100 (resistant genotype. The genotypes CR-1, CR-3, Davis and Cristalina under low level of infestation (2.8 Heteroptera/beating produced similar percentage of normal seeds (57% but inferior to the genotype IAC-100 (77%. Under high level of infestation (6.42 Heteroptera/beating, the genotypes CR-1, CR-3 and Cristalina produced

  5. The Purification of a Blood Group A Glycoprotein: An Affinity Chromatography Experiment.

    Science.gov (United States)

    Estelrich, J.; Pouplana, R.

    1988-01-01

    Describes a purification process through affinity chromatography necessary to obtain specific blood group glycoproteins from erythrocytic membranes. Discusses the preparation of erythrocytic membranes, extraction of glycoprotein from membranes, affinity chromatography purification, determination of glycoproteins, and results. (CW)

  6. Microcystin Detection Characteristics of Fluorescence Immunochromatography and High Performance Liquid Chromatography

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Park, Geun Young; Choi, Jong Chon; Oh, Chang Suk

    2005-01-01

    Different detection characteristics of fluorescence immunochromatography method and high performance liquid chromatography (HPLC) method for the analysis of cyanobacterial toxins were studied. In particular, low and high limits of detection, detection time and reproducibility and detectable microcystin species were compared when fluorescence immunochromatography method and high performance liquid chromatography method were applied for the detection of microcystin (MC), a cyclic peptide toxin of the freshwater cyanobacterium Microcystis aeruginosa. A Fluorescence immunochromatography assay system has the unique advantages of short detection time and low detection limit, and high performance liquid chromatography detection method has the strong advantage of individual quantifications of several species of microcystins

  7. High-Performance Liquid Chromatography-Mass Spectrometry.

    Science.gov (United States)

    Vestal, Marvin L.

    1984-01-01

    Reviews techniques for online coupling of high-performance liquid chromatography with mass spectrometry, emphasizing those suitable for application to nonvolatile samples. Also summarizes the present status, strengths, and weaknesses of various techniques and discusses potential applications of recently developed techniques for combined liquid…

  8. Intercomparison of the measurements of oxalic acid in aerosols by gas chromatography and ion chromatography

    Science.gov (United States)

    Kawamura, Kimitaka; Barrie, Leonard A.; Toom-Sauntry, Desiree

    2010-12-01

    Oxalate, the anion of oxalic acid, is one of the most abundant measurable organic species in atmospheric aerosols. Traditionally, this bifunctional species has been measured by gas chromatography (GC) after derivatization to butyl ester and by ion chromatography (IC) without derivatization. However, there are few published comparisons of the two techniques. Here, we report the results of an intercomparison study for the measurement of oxalic acid in Arctic aerosols (oxalic acid by GC ranged from 6.5-59.1 ng m -3 (av. 26.0 ng m -3, median 26.2 ng m -3) whereas those by IC ranged from 6.6-52.1 ng m -3 (av. 26.6 ng m -3, median 25.4 ng m -3). They showed a good correlation ( r = 0.84) with a slope of 0.96. Thus, observations of oxalate obtained by GC employing dibutyl esters are almost equal to those by IC. Because the accuracy of oxalic acid by GC method largely depends on the method used, it is important to strictly examine the recovery in each study.

  9. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

    HP

    Original Research Article. Gas Chromatography-Mass Spectrometric Analysis and ... into a natural fumigant/insecticide for the control of stored product insects. Keywords: Mallotus ..... stability as well as reduce cost. ACKNOWLEDGEMENT.

  10. Boron isotopic enrichment by displacement chromatography

    International Nuclear Information System (INIS)

    Mohapatra, K.K.; Bose, Arun

    2014-01-01

    10 B enriched boron is used in applications requiring high volumetric neutron absorption (absorption cross section- 3837 barn for thermal and 1 barn for 1 MeV fast neutron). It is used in fast breeder reactor (as control rod material), in neutron counter, in Boron Neutron Capture Therapy etc. Owing to very small separation factor, boron isotopic enrichment is a complex process requiring large number of separation stages. Heavy Water Board has ventured in industrial scale production of 10 B enriched boron using Exchange Distillation Process as well as Ion Displacement Chromatography Process. Ion Displacement Chromatography process is used in Boron Enrichment Plant at HWP, Manuguru. It is based on isotopic exchange between borate ions (B(OH) 4 - ) on anion exchange resin and boric acid passing through resin. The isotopic exchange takes place due to difference in zero point energy of 10 B and 11 B

  11. Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

    Science.gov (United States)

    Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

    2017-10-13

    A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Exploration of overloaded cation exchange chromatography for monoclonal antibody purification.

    Science.gov (United States)

    Liu, Hui F; McCooey, Beth; Duarte, Tiago; Myers, Deanna E; Hudson, Terry; Amanullah, Ashraf; van Reis, Robert; Kelley, Brian D

    2011-09-28

    Cation exchange chromatography using conventional resins, having either diffusive or perfusive flow paths, operated in bind-elute mode has been commonly employed in monoclonal antibody (MAb) purification processes. In this study, the performance of diffusive and perfusive cation exchange resins (SP-Sepharose FF (SPSFF) and Poros 50HS) and a convective cation exchange membrane (Mustang S) and monolith (SO(3) Monolith) were compared. All matrices were utilized in an isocratic state under typical binding conditions with an antibody load of up to 1000 g/L of chromatographic matrix. The dynamic binding capacity of the cation exchange resins is typically below 100 g/L resin, so they were loaded beyond the point of anticipated MAb break through. All of the matrices performed similarly in that they effectively retained host cell protein and DNA during the loading and wash steps, while antibody flowed through each matrix after its dynamic binding capacity was reached. The matrices differed, though, in that conventional diffusive and perfusive chromatographic resins (SPSFF and Poros 50HS) demonstrated a higher binding capacity for high molecular weight species (HMW) than convective flow matrices (membrane and monolith); Poros 50HS displayed the highest HMW binding capacity. Further exploration of the conventional chromatographic resins in an isocratic overloaded mode demonstrated that the impurity binding capacity was well maintained on Poros 50HS, but not on SPSFF, when the operating flow rate was as high as 36 column volumes per hour. Host cell protein and HMW removal by Poros 50HS was affected by altering the loading conductivity. A higher percentage of host cell protein removal was achieved at a low conductivity of 3 mS/cm. HMW binding capacity was optimized at 5 mS/cm. Our data from runs on Poros 50HS resin also showed that leached protein A and cell culture additive such as gentamicin were able to be removed under the isocratic overloaded condition. Lastly, a MAb

  13. Application of ion chromatography in clinical studies and pharmaceutical industry.

    Science.gov (United States)

    Michalski, Rajmund

    2014-01-01

    Ion chromatography is a well-established regulatory method for analyzing anions and cations in environmental, food and many other samples. It offers an enormous range of possibilities for selecting stationary and mobile phases. Additionally, it usually helps to solve various separation problems, particularly when it is combined with different detection techniques. Ion chromatography can also be used to determine many ions and substances in clinical and pharmaceutical samples. It provides: availability of high capacity stationary phases and sensitive detectors; simple sample preparation; avoidance of hazardous chemicals; decreased sample volumes; flexible reaction options on a changing sample matrix to be analyzed; or the option to operate a fully-automated system. This paper provides a short review of the ion chromatography applications for determining different inorganic and organic substances in clinical and pharmaceutical samples.

  14. State-of-the art of selective detection and identification of I-, Br-, Cl-, and F-containing compounds in gas chromatography and liquid chromatography.

    Science.gov (United States)

    Brede, Cato; Pedersen-Bjergaard, Stig

    2004-09-24

    This review article presents an overview of halogen-specific detection in gas chromatography (GC) and liquid chromatography (LC). Attention is primarily focused on the use of plasma emission spectroscopy and plasma mass spectrometry as detectors, but other halogen-selective detection principles are also mentioned. Different instrumental configurations are discussed both with respect to technical set-up and performance, the principal reasons for halogen-selective detection are highlighted, and recent applications are reviewed from areas such as environmental chemistry, petroleum characterization, and drug analysis.

  15. Screening antiallergic components from Carthamus tinctorius using rat basophilic leukemia 2H3 cell membrane chromatography combined with high-performance liquid chromatography and tandem mass spectrometry.

    Science.gov (United States)

    Han, Shengli; Huang, Jing; Cui, Ronghua; Zhang, Tao

    2015-02-01

    Carthamus tinctorius, used in traditional Chinese medicine, has many pharmacological effects, such as anticoagulant effects, antioxidant effects, antiaging effects, regulation of gene expression, and antitumor effects. However, there is no report on the antiallergic effects of the components in C. tinctorius. In the present study, we investigated the antiallergic components of C. tinctorius and its mechanism of action. A rat basophilic leukemia 2H3/cell membrane chromatography coupled online with high-performance liquid chromatography and tandem mass spectrometry method was developed to screen antiallergic components from C. tinctorius. The screening results showed that Hydroxysafflor yellow A, from C. tinctorius, was the targeted component that retained on the rat basophilic leukemia 2H3/cell membrane chromatography column. We measured the amount of β-hexosaminidase and histamine released in mast cells and the key markers of degranulation. The release assays showed that Hydroxysafflor yellow A could attenuate the immunoglobulin E induced release of allergic cytokines without affecting cell viability from 1.0 to 50.0 μM. In conclusion, the established rat basophilic leukemia 2H3 cell membrane chromatography coupled with online high-performance liquid chromatography and tandem mass spectrometry method successfully screened and identified Hydroxysafflor yellow A from C. tinctorius as a potential antiallergic component. Pharmacological analysis elucidated that Hydroxysafflor yellow A is an effective natural component for inhibiting immunoglobulin E-antigen-mediated degranulation. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. A Narrow Internal Auditory Canal with Duplication in a Patient with Congenital Sensorineural Hearing Loss

    Energy Technology Data Exchange (ETDEWEB)

    Baik, Hye Won; Yu, Hye On; Kim, Kyung Soo; Kim, Gi Hyeon [Chung-Ang University Hospital, College of Medicine, Seoul (Korea, Republic of)

    2008-07-15

    A narrow internal auditory canal (IAC) with duplication is a rare anomaly of the temporal bone. It is associated with congenital sensorineural hearing loss. Aplasia or hypoplasia of the vestibulocochlear nerve may cause the hearing loss. We present an unusual case of an isolated narrow IAC with duplication that was detected by a CT scan. In this case, the IAC was divided by a bony septum into an empty stenotic inferoposterior portion and a large anterosuperior portion containing the facial nerve that was clearly delineated on MRI.

  17. Radiochemical purity determination by paper chromatography 2

    International Nuclear Information System (INIS)

    1975-01-01

    The standard relates to the determination of radiochemical impurities in labelled compounds using paper chromatography. The basic terms are given as is the description of procedure and evaluation of chromatograms. (E.S.)

  18. Gas Chromatography-Mass Spectrometric Analysis of Nematicidal ...

    African Journals Online (AJOL)

    Gas Chromatography-Mass Spectrometric Analysis of Nematicidal Essential Oil of Valeriana ... Tropical Journal of Pharmaceutical Research ... have a potential to be developed to natural nematicides for the control of cereal cyst nematodes.

  19. Comparison of different transition metal ions for immobilized metal affinity chromatography of selenoprotein P from human plasma

    DEFF Research Database (Denmark)

    Sidenius, U; Farver, O; Jøns, O

    1999-01-01

    Cu2+, Ni2+, Zn2+, Co2+ and Cd2+ were evaluated in metal ion affinity chromatography for enrichment of selenoprotein P, and immobilized Co2+ affinity chromatography was found to be the most selective chromatographic method. The chromatography was performed by fast protein liquid chromatography...

  20. Potential application of gas chromatography to the analysis of hydrogen isotopes

    International Nuclear Information System (INIS)

    Warner, D.K.; Sprague, R.E.; Bohl, D.R.

    1976-01-01

    Gas chromatography is used at Mound Laboratory for the analysis of hydrogen isotopic impurities in gas mixtures. This instrumentation was used to study the applicability of the gas chromatography technique to the determination of the major components of hydrogen isotopic gas mixtures. The results of this study, including chromatograms and precision data, are presented

  1. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... apelta aerial parts was analyzed by gas chromatography/mass spectrometric (GC/MS) to determine its composition. ... into a natural fumigant/insecticide for the control of stored product insects.

  2. Identification of Cyclopentenyl Fatty Acids by Gas Liquid Chromatography and Mass Spectrometry

    DEFF Research Database (Denmark)

    Shukla, V. K. S.; Abdel-Moety, E. M.; Larsen, Elfinn

    1979-01-01

    The straight chain fatty acids and the cyclopentenyl fatty acids present in the lipids of Hydnocarpus wightiana seeds were separated as their pyrrolidides by means of gas chromatography. A gas chromatography-mass spectrometry system confirmed the complete separation and permitted the identification...

  3. Early stages in the history of gas chromatography.

    Science.gov (United States)

    Kolomnikov, Ivan G; Efremov, Alexander M; Tikhomirova, Tatyana I; Sorokina, Nadezhda M; Zolotov, Yury A

    2018-02-16

    The creation of gas chromatography is traditionally associated with the names of Nobel Prize winner Archer Martin and his colleagues Richard Synge and Anthony James. However, sometimes references to their predecessors can be found. An investigation conducted by the authors of this article not only confirmed the reliability of these references; but in fact led to the conclusion that by 1952, which is commonly believed to be the year when gas chromatography was born, many research papers had already been devoted to this method, mainly, in its gas-solid version. These papers are considered in this article. Copyright © 2018. Published by Elsevier B.V.

  4. Column liquid chromatography applied to concentrating, separating, and determining platinum metals

    International Nuclear Information System (INIS)

    Alimarin, I.P.; Basova, E.M.; Bol'shova, T.A.; Ivanov, V.M.

    1986-01-01

    The present survey deals with high-performance liquid chromatography (HPLC) in relation to the chromatographic behavior of the platinum metals, including separation and determination. The data shows that HPLC is the most promising and effective method of separating metals, including platinum ones. The method provides efficient separation of microgram amoounts of mixtures with a resolving power 3-20 times that of thin-layer chromatography. It is shown that the most promising line of advance in HPLC for inorganic systems lies in the separation and determination of metals as chelates by absorption or ion-pair chromatography. Examples of using HPLC for determining noble metals in particular cases indicate that the metrological characteristics are favorable

  5. Ion exclusion chromatography for the purification of L-glutamine; Ion haijo chromatography ni yoru L-glutamine no seiseiho no kenkyu

    Energy Technology Data Exchange (ETDEWEB)

    Ito, H.; Nishi, A.; Naruse, M. [Ajinomoto Co. Inc., Kawasaki (Japan)

    1998-09-05

    Ion exclusion chromatography for the purification of L-glutamine is studied. L-glutamine is usually produced by fermentation and used in pharmaceuticals. By using a model solution of L-glutamine and L-glutamic acid, the optimum cation exchange resin is examined. As a result of the experiments, it is found that a cation exchange resin which has smaller crosslinkage and smaller diameter is better. Ammonium sulfate, L-glutamic acid and pyrrolidonecarboxylic acid, which are usually contained in fermentation broth as impurities, are effectively separated by this method. Moreover, the experimental data of the chromatography is expressed fairly well by the differential equations which express the mass transfer in the fixed bed. 8 refs., 5 figs., 2 tabs.

  6. Analysis of short-chain acids from anaerobic bacteria by high-performance liquid chromatography.

    OpenAIRE

    Guerrant, G O; Lambert, M A; Moss, C W

    1982-01-01

    A standard mixture of 25 short-chain fatty acids was resolved by high-performance liquid chromatography, using an Aminex HPX-87 column. The acids produced in culture media by anaerobic bacteria were analyzed by high-performance liquid chromatography after extraction with ether and reextraction into a small volume of 0.1 N NaOH. The presence of fumaric acid in culture extracts of Peptostreptococcus anaerobius was confirmed by gas chromatography-mass spectrometry analysis of the trapped eluent ...

  7. Intra-arterial chemotherapy for retinoblastoma: First Indian report

    Directory of Open Access Journals (Sweden)

    Pukhraj Rishi

    2015-01-01

    Full Text Available Aim: To describe treatment outcomes and complications of selective intra-arterial chemotherapy (IAC for retinoblastoma (RB in Indian eyes. Materials and Methods: Single center, retrospective interventional case series of 6 eyes with RB who underwent IAC using Melphalan (3 mg/5 mg/7.5 mg and topetecan (1 mg (n = 4 or melphalan (3 mg/5 mg/7.5 mg alone (n = 2 between December 2013 and June 2014. In all, 17 IAC procedures were performed using selective ophthalmic artery cannulation. Treatment outcomes were evaluated in terms of tumor control, vitreous and subretinal seeds control and globe salvage rates. Results: IAC was employed as primary (n = 1 or secondary (n = 5 modality of treatment. Each eye received mean 3 IAC sessions (median: 3; range: 1-4 sessions. Eyes were classified according to international classification of RB as Group B (n = 1, C (n = 1, D (n = 2 and E (n = 2. Following IAC, complete regression of the main tumor was seen in 3 cases (50%, partial regression in 2 (33%, while 1 case (15% showed no response. Of 4 eyes with subretinal seeds, 1 (25% eye had complete regression while 3 (75% eyes had partial regression. Of 5 eyes with vitreous seeds, 2 (40% eyes had complete regression while 3 (60% eyes had a partial response. Globe salvage was achieved in 5 of 6 eyes (83%. Diffuse choroidal atrophy and vitreous hemorrhage were observed in 1 (17% eye, each. No hematologic toxicity or cerebro-vascular events were observed. Mean follow-up period was 5.5 months (median: 6 months, range: 1-6 months. Conclusion: IAC is an effective therapy for globe preservation in eyes with RB. Larger studies with longer follow-up are required to validate these results.

  8. Two-group interfacial area concentration correlations of two-phase flows in large diameter pipes

    International Nuclear Information System (INIS)

    Shen, Xiuzhong; Hibiki, Takashi

    2015-01-01

    The reliable empirical correlations and models are one of the important ways to predict the interfacial area concentration (IAC) in two-phase flows. However, up to now, no correlation or model is available for the prediction of the IAC in the two-phase flows in large diameter pipes. This study collected an IAC experimental database of two-phase flows taken under various flow conditions in large diameter pipes and presented a systematic way to predict the IAC for two-phase flows from bubbly, cap-bubbly to churn flow in large diameter pipes by categorizing bubbles into two groups (group-1: spherical and distorted bubble, group-2: cap bubble). Correlations were developed to predict the group-1 void fraction from the void fraction of all bubble. The IAC contribution from group-1 bubbles was modeled by using the dominant parameters of group-1 bubble void fraction and Reynolds number based on the parameter-dependent analysis of Hibiki and Ishii (2001, 2002) using one-dimensional bubble number density and interfacial area transport equations. A new drift velocity correlation for two-phase flow with large cap bubbles in large diameter pipes was derived in this study. By comparing the newly-derived drift velocity correlation with the existing drift velocity correlation of Kataoka and Ishii (1987) for large diameter pipes and using the characteristics of the representative bubbles among the group 2 bubbles, we developed the model of IAC and bubble size for group 2 cap bubbles. The developed models for estimating the IAC are compared with the entire collected database. A reasonable agreement was obtained with average relative errors of ±28.1%, ±54.4% and ±29.6% for group 1, group 2 and all bubbles respectively. (author)

  9. Cortical integrity of the inferior alveolar canal as a predictor of paresthesia after third-molar extraction.

    Science.gov (United States)

    Park, Wonse; Choi, Ji-Wook; Kim, Jae-Young; Kim, Bong-Chul; Kim, Hyung Jun; Lee, Sang-Hwy

    2010-03-01

    Paresthesia is a well-known complication of extraction of mandibular third molars (MTMs). The authors evaluated the relationship between paresthesia after MTM extraction and the cortical integrity of the inferior alveolar canal (IAC) by using computed tomography (CT). The authors designed a retrospective cohort study involving participants considered, on the basis of panoramic imaging, to be at high risk of experiencing injury of the inferior alveolar nerve who subsequently underwent CT imaging and extraction of the MTMs. The primary predictor variable was the contact relationship between the IAC and the MTM as viewed on a CT image, classified into three groups: group 1, no contact; group 2, contact between the MTM and the intact IAC cortex; group 3, contact between the MTM and the interrupted IAC cortex. The secondary predictor variable was the number of CT image slices showing the cortical interruption around the MTM. The outcome variable was the presence or absence of postoperative paresthesia after MTM extraction. The study sample comprised 179 participants who underwent MTM extraction (a total of 259 MTMs). Their mean age was 23.6 years, and 85 (47.5 percent) were male. The overall prevalence of paresthesia was 4.2 percent (11 of 259 teeth). The prevalence of paresthesia in group 3 (involving an interrupted IAC cortex) was 11.8 percent (10 of 85 cases), while for group 2 (involving an intact IAC cortex) and group 1 (involving no contact) it was 1.0 percent (1 of 98 cases) and 0.0 percent (no cases), respectively. The frequency of nerve damage increased with the number of CT image slices showing loss of cortical integrity (P=.043). The results of this study indicate that loss of IAC cortical integrity is associated with an increased risk of experiencing paresthesia after MTM extraction.

  10. GENETIC DIVERSITY IN ARABICA COFFEE GROWN IN POTASSIUM-CONSTRAINED ENVIRONMENT

    Directory of Open Access Journals (Sweden)

    Waldênia de Melo Moura

    2015-02-01

    Full Text Available Potassium is a source of non-renewable natural resource, and is used in large quantities in coffee fertilization through basically imported formulations in the form of potassium chloride. An alternative to make production systems more sustainable would be obtaining cultivars more efficient in the use of this nutrient. This study aimed to evaluate the genetic diversity among 20 cultivars of coffee, in conditions of low availability of potassium to identify the best combinations for composing future populations to be used in breeding programs. The experiment was arranged in a randomized block design with three replications of nutrient solution. Agronomic characteristics and efficiencies of rooting, absorption, translocation, biomass production and potassium utilization were evaluated. The clustering analysis was based on the unweighted pair group method with arithmetic mean clustering algorithm (UPGMA and canonical variables. Variability was observed for most treatments. The multivariate procedures produced similar discrimination of genotypes, with the formation of five groups. Hybridizations between the cultivar Icatu Precoce IAC 3283 with cultivars Catuaí Amarelo IAC 62, Araponga MG1, Caturra Vermelho IAC 477, Catuaí Vermelho IAC 15, Rubi MG 1192 and Catucaí 785/15, and between the cultivar Tupi IAC 1669-33 with cultivars Icatu Vermelho IAC 4045, Acaiá Cerrado MG 1474 and Oeiras MG 6851 are the most promising for obtaining segregating populations or heterotic hybrids in breeding programs aiming more efficiency in potassium utilization.

  11. Development of the interfacial area concentration measurement method using a five sensor conductivity probe

    International Nuclear Information System (INIS)

    Euh, Dong Jin; Yun, Byong Jo; Song, Chul Hwa; Kwon, Tae Soon; Chung, Moon Ki; Lee, Un Chul

    2000-01-01

    The interfacial area concentration(IAC) is one of the most important parameters in the two-fluid model for two-phase flow analysis. The IAE can be measured by a local conductivity probe method that uses the difference of conductivity between water and air/steam. The number of sensors in the conductivity probe may be differently chosen by considering the flow regime of two-phase flow. The four sensor conductivity probe method predicts the IAC without any assumptions of the bubble shape. The local IAC can be obtained by measuring the three dimensional velocity vector elements at the measuring point, and the directional cosines of the sensors. The five sensor conductivity probe method proposed in this study is based on the four sensor probe method. With the five sensor probe, the local IAC for a given referred measuring area of the probe can be predicted more exactly than the four sensor prober. In this paper, the mathematical approach of the five sensor probe method for measuring the IAC is described, and a numerical simulation is carried out for ideal cap bubbles of which the sizes and locations are determined by a random number generator

  12. Triticonazole enantiomers: Separation by supercritical fluid chromatography and the effect of the chromatographic conditions.

    Science.gov (United States)

    He, Jianfeng; Fan, Jun; Yan, Yilun; Chen, Xiaodong; Wang, Tai; Zhang, Yaomou; Zhang, Weiguang

    2016-11-01

    Enantiomeric pairs of triticonazole have been successfully separated by supercritical fluid chromatography coupled with a tris(3,5-dimethylphenylcarbamoyl) cellulose-coated chiral stationary phase in this work. The effects of co-solvent, dissolution solvent, flow rate, backpressure, and column temperature have been studied in detail with respect to retention, selectivity, and resolution of triticonazole. As indicated, the co-solvents mostly affected the retention factors and resolution, due to the different molecular structure and polarity. In addition, the dissolution solvents, namely, chloromethanes and alcohols, have been also important for enantioseparation because of the different interaction with stationary phase. Higher flow rate and backpressure led to faster elution of the triticonazole molecules, and the change of column temperature showed slight effect on the resolution of triticonazole racemate. Moreover, a comparative separation experiment between supercritical fluid chromatography and high performance liquid chromatography revealed that chiral supercritical fluid chromatography gave the 3.5 times value of R s /t R2 than high performance liquid chromatography, which demonstrated that supercritical fluid chromatography had much higher separation efficiency. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  13. Trends in data processing of comprehensive two-dimensional chromatography: state of the art.

    Science.gov (United States)

    Matos, João T V; Duarte, Regina M B O; Duarte, Armando C

    2012-12-01

    The operation of advanced chromatographic systems, namely comprehensive two-dimensional (2D) chromatography coupled to multidimensional detectors, allows achieving a great deal of data that need special care to be processed in order to characterize and quantify as much as possible the analytes under study. The aim of this review is to identify the main trends, research needs and gaps on the techniques for data processing of multidimensional data sets obtained from comprehensive 2D chromatography. The following topics have been identified as the most promising for new developments in the near future: data acquisition and handling, peak detection and quantification, measurement of overlapping of 2D peaks, and data analysis software for 2D chromatography. The rational supporting most of the data processing techniques is based on the generalization of one-dimensional (1D) chromatography although algorithms, such as the inverted watershed algorithm, use the 2D chromatographic data as such. However, for processing more complex N-way data there is a need for using more sophisticated techniques. Apart from using other concepts from 1D chromatography, which have not been tested for 2D chromatography, there is still room for new improvements and developments in algorithms and software for dealing with 2D comprehensive chromatographic data. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Forced-flow chromatography of rare earths using sensitive spectrophometry

    International Nuclear Information System (INIS)

    Matsui, Masakazu; Aoki, Toru; Kumagai, Tetsu.

    1981-01-01

    The sensitive spectrophotometric method for the rare earth elements with xylenol orange in the presence of cetylpyridinium bromide was applied to the continuous detection system of liquid chromatography. Fourteen rare earth elements were completely separated within 130 min cation-exchange chromatography using 2-hydroxy-iso-butylic acid. The eluted ions were determined with absorption maxima of their complexes at around 610 nm. A linear relationship between the peak height and the amounts of rare earth elements was also obtained over the range 0.04 to 0.5 MU g. (author)

  15. Study of comportment of trioctylphosphine oxide by coat slight chromatography

    International Nuclear Information System (INIS)

    Meddour, Laaldja; Azzouz Abdelkrim

    1996-04-01

    The synthesis and characterisation process of the extractant agent 'Trioctylphosphine oxide' (TOPO) are not very developped in the literature. However, in order to identify this agent (TOPO) in its synthesis process, we attempt several analysis methods. The coat slight chromatography proves the simple and accessible method, that explains the choice of this study. In the present work, we have analysed the TOPO by coat slight chromatography with the intention of finding a better solvent

  16. Hyphenated techniques in multidimensional gas chromatography for analysis of wine aroma and related odorants

    OpenAIRE

    Chin, Sung Tong

    2017-01-01

    The advent of analytical multidimensional gas chromatography (MDGC) techniques, with recent development in comprehensive two-dimensional gas chromatography (GC×GC) as well as microfluidic technology in conventional heart-cut MDGC, has achieved excellent separation efficiency for advanced characterization of complex volatile and semi-volatile samples, which is unlikely to be accomplished by single dimensional chromatography. This dissertation work has highlighted the potential opportunities fo...

  17. Electronic spectral detection in liquid chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Biggs, Wilton R. [ChevronTexaco Chemical Co., P. O. Box 1627, Richmond, CA 94802 (United States); Fetzer, John C. [Fetzpahs Consulting, 1283 Santa Fe St., Hercules, CA 94547 (United States)

    2002-07-01

    The use of absorbance and fluorescence spectrometers as liquid chromatography detectors is described. These detectors offer sensitive detection that can also identify the peaks in a chromatogram. Many examples, mainly from the separation of polycyclic aromatic hydrocarbons, are given that show the selectivity and usefulness of these detectors. (orig.)

  18. Analytical biotechnology: Capillary electrophoresis and chromatography

    International Nuclear Information System (INIS)

    Horvath, C.; Nikelly, J.G.

    1990-01-01

    The papers describe the separation, characterization, and equipment required for the electrophoresis or chromatography of cyclic nucleotides, pharmaceuticals, therapeutic proteins, recombinant DNA products, pheromones, peptides, and other biological materials. One paper, On-column radioisotope detection for capillary electrophoresis, has been indexed separately for inclusion on the data base

  19. Size-exclusion chromatography for the determination of the boiling point distribution of high-boiling petroleum fractions.

    Science.gov (United States)

    Boczkaj, Grzegorz; Przyjazny, Andrzej; Kamiński, Marian

    2015-03-01

    The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range distribution by chromatography has been accomplished using simulated distillation with gas chromatography with flame ionization detection. This study revealed that in spite of substantial differences in the separation mechanism and the detection mode, the size-exclusion chromatography technique yields similar results for the determination of boiling point distribution compared with simulated distillation and novel empty column gas chromatography. The developed procedure using size-exclusion chromatography has a substantial applicability, especially for the determination of exact final boiling point values for high-boiling mixtures, for which a standard high-temperature simulated distillation would have to be used. In this case, the precision of final boiling point determination is low due to the high final temperatures of the gas chromatograph oven and an insufficient thermal stability of both the gas chromatography stationary phase and the sample. Additionally, the use of high-performance liquid chromatography detectors more sensitive than refractive index detection allows a lower detection limit for high-molar-mass aromatic compounds, and thus increases the sensitivity of final boiling point determination. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Science.gov (United States)

    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.

  1. Advances in silver ion chromatography for the analysis of fatty acids and triacylglycerols-2001 to 2011.

    Science.gov (United States)

    Momchilova, Svetlana M; Nikolova-Damyanova, Boryana M

    2012-01-01

    An effort is made to critically present the achievements in silver ion chromatography during the last decade. Novelties in columns, mobile-phase compositions and detectors are described. Recent applications of silver ion chromatography in the analysis of fatty acids and triacylglycerols are presented while stressing novel analytical strategies or new objects. The tendencies in the application of the method in complementary ways with reversed-phase chromatography, chiral chromatography and, especially, mass detection are outlined.

  2. Pressurized planar electrochromatography, high-performance thin-layer chromatography and high-performance liquid chromatography--comparison of performance.

    Science.gov (United States)

    Płocharz, Paweł; Klimek-Turek, Anna; Dzido, Tadeusz H

    2010-07-16

    Kinetic performance, measured by plate height, of High-Performance Thin-Layer Chromatography (HPTLC), High-Performance Liquid Chromatography (HPLC) and Pressurized Planar Electrochromatography (PPEC) was compared for the systems with adsorbent of the HPTLC RP18W plate from Merck as the stationary phase and the mobile phase composed of acetonitrile and buffer solution. The HPLC column was packed with the adsorbent, which was scrapped from the chromatographic plate mentioned. An additional HPLC column was also packed with adsorbent of 5 microm particle diameter, C18 type silica based (LiChrosorb RP-18 from Merck). The dependence of plate height of both HPLC and PPEC separating systems on flow velocity of the mobile phase and on migration distance of the mobile phase in TLC system was presented applying test solute (prednisolone succinate). The highest performance, amongst systems investigated, was obtained for the PPEC system. The separation efficiency of the systems investigated in the paper was additionally confirmed by the separation of test component mixture composed of six hormones. 2010 Elsevier B.V. All rights reserved.

  3. Increased biological activity of deglycosylated recombinant human granulocyte/macrophage colony-stimulating factor produced by yeast or animal cells

    International Nuclear Information System (INIS)

    Moonen, P.; Mermod, J.J.; Ernst, J.F.; Hirschi, M.; DeLamarter, J.F.

    1987-01-01

    Human granulocyte/macrophage colony-stimulating factor (hGM-CSF) produced by several recombinant sources including Escherichia coli, yeast, and animal cells was studied. Recombinant animal cells produced hGM-CSF in low quantities and in multiple forms of varying size. Mammalian hGM-CSF was purified 200,000-fold using immunoaffinity and lectin chromatography. Partially purified proteins produced in yeast and mammalian cells were assayed for the effects of deglycosylation. Following enzymatic deglycosylation, immunoreactivity was measured by radioimmunoassay and biological activity was measured in vitro on responsive human primary cells. Removal of N-linked oligosaccharides from both proteins increased their immunoreactivities by 4- to 8-fold. Removal of these oligosaccharides also increased their specific biological activities about 20-fold, to reach approximately the specific activity of recombinant hGM-CSF from E. coli. The E. coli produced-protein-lacking any carbohydrate- had by far the highest specific activity observed for the recombinant hGM-CSFs

  4. NovaSil clay intervention in Ghanaians at high risk for aflatoxicosis: II. Reduction in biomarkers of aflatoxin exposure in blood and urine.

    Science.gov (United States)

    Wang, P; Afriyie-Gyawu, E; Tang, Y; Johnson, N M; Xu, L; Tang, L; Huebner, H J; Ankrah, N-A; Ofori-Adjei, D; Ellis, W; Jolly, P E; Williams, J H; Wang, J-S; Phillips, T D

    2008-05-01

    The efficacy of NovaSil clay (NS) to reduce aflatoxin (AF) biomarkers of exposure was evaluated in 656 blood samples and 624 urine samples collected from study participants during a 3-month phase IIa clinical intervention trial in Ghana. NS was delivered before meals via capsules. Serum AFB (1)-albumin adduct was measured by radioimmunoassay and urinary AFM (1) metabolites were quantified by immunoaffinity-high-performance liquid chromatography (HPLC)-fluorescence methods. Levels of AFB (1) -albumin adduct in serum samples collected at baseline and at 1 month were similar (p = 0.2354 and p = 0.3645, respectively) among the placebo (PL), low dose (LD, 1.5 g NS day (-1)), and high dose (HD, 3.0 g NS day (-1)) groups. However, the levels of AFB (1)-albumin adduct at 3 months were significantly decreased in both the LD group (p clay can be used to reduce effectively the bioavailability of dietary AF based on a reduction of AF-specific biomarkers.

  5. Natural postharvest aflatoxin occurrence in food legumes in the smallholder farming sector of Zimbabwe.

    Science.gov (United States)

    Maringe, David Tinayeshe; Chidewe, Cathrine; Benhura, Mudadi Albert; Mvumi, Brighton Marimanzi; Murashiki, Tatenda Clive; Dembedza, Mavis Precious; Siziba, Lucia; Nyanga, Loveness Kuziwa

    2017-03-01

    Aflatoxins, mainly produced by Aspergillus flavus and Aspergillus parasiticus, are highly toxic and may lead to health problems such as liver cancer. Exposure to aflatoxins may result from ingestion of contaminated foods. Levels of AFB 1 , AFB 2 , AFG 1 and AFG 2 in samples of groundnuts (Arachis hypogaea), beans (Phaseolus vulgaris), cowpeas (Vigna unguiculata) and bambara nuts (Vigna subterranean) grown by smallholder farmers in Shamva and Makoni districts, Zimbabwe, were determined at harvesting, using high performance liquid chromatography after immunoaffinity clean-up. Aflatoxins were detected in 12.5% of groundnut samples with concentrations ranging up to 175.9 µg/kg. Aflatoxins were present in 4.3% of the cowpea samples with concentrations ranging from 1.4 to 103.4 µg/kg. Due to alarming levels of aflatoxins detected in legumes versus maximum permissible levels, there is a need to assist smallholder farmers to develop harvest control strategies to reduce contamination of aflatoxins in legumes.

  6. Proteomic Profile of Unstable Atheroma Plaque: Increased Neutrophil Defensin 1, Clusterin, and Apolipoprotein E Levels in Carotid Secretome.

    Science.gov (United States)

    Aragonès, Gemma; Auguet, Teresa; Guiu-Jurado, Esther; Berlanga, Alba; Curriu, Marta; Martinez, Salomé; Alibalic, Ajla; Aguilar, Carmen; Hernández, Esteban; Camara, María-Luisa; Canela, Núria; Herrero, Pol; Ruyra, Xavier; Martín-Paredero, Vicente; Richart, Cristóbal

    2016-03-04

    Because of the clinical significance of carotid atherosclerosis, the search for novel biomarkers has become a priority. The aim of the present study was to compare the protein secretion profile of the carotid atherosclerotic plaque (CAP, n = 12) and nonatherosclerotic mammary artery (MA, n = 10) secretomes. We used a nontargeted proteomic approach that incorporated tandem immunoaffinity depletion, iTRAQ labeling, and nanoflow liquid chromatography coupled to high-resolution mass spectrometry. In total, 162 proteins were quantified, of which 25 showed statistically significant differences in secretome levels between carotid atherosclerotic plaque and nondiseased mammary artery. We found increased levels of neutrophil defensin 1, apolipoprotein E, clusterin, and zinc-alpha-2-glycoprotein in CAP secretomes. Results were validated by ELISA assays. Also, differentially secreted proteins are involved in pathways such as focal adhesion and leukocyte transendothelial migration. In conclusion, this study provides a subset of identified proteins that are differently expressed in secretomes of clinical significance.

  7. Effects of Bread Making and Wheat Germ Addition on the Natural Deoxynivalenol Content in Bread

    Science.gov (United States)

    Giménez, Isabel; Blesa, Jesús; Herrera, Marta; Ariño, Agustín

    2014-01-01

    Deoxynivalenol (DON, vomitoxin) is a type-B trichothecene mycotoxin produced by several field fungi such as Fusarium graminearum and Fusarium culmorum and known to have various toxic effects. This study investigated the effect of the bread making process on the stability of DON in common bread and wheat germ-enriched bread using naturally contaminated ingredients at the level of 560 µg/kg. The concentration of DON and its evolution during bread making were determined by immunoaffinity column cleanup followed by liquid chromatography with diode array detection (HPLC-DAD). During the bread making process, DON was reduced by 2.1% after fermentation and dropped by 7.1% after baking, reaching a maximum reduction of 19.8% in the crust as compared with a decrease of 5.6% in the crumb. The addition of 15% wheat germ to the dough did not affect DON stability during bread making, showing an apparent increase of 3.5% after fermentation and a reduction by 10.2% after baking. PMID:24451845

  8. Occurrence of ochratoxin A in cocoa by-products and determination of its reduction during chocolate manufacture.

    Science.gov (United States)

    Copetti, Marina V; Iamanaka, Beatriz T; Nester, Melanie A; Efraim, Priscilla; Taniwaki, Marta H

    2013-01-01

    This work reports an investigation carried out to assess the natural occurrence of ochratoxin A in 168 samples from different fractions obtained during the technological processing of cocoa (shell, nibs, liquor, butter, cake and cocoa powder) and the reduction of ochratoxin A during chocolate manufacture. Ochratoxin A analyses were performed with immunoaffinity columns and detection by high performance liquid chromatography. Concerning the natural ochratoxin A contamination in cocoa by-products, the highest levels of ochratoxin A were found in the shell, cocoa powder and cocoa cake. The cocoa butter was the least contaminated, showing that ochratoxin A seems to remain in the defatted cocoa solids. Under the technological conditions applied during the manufacture of chocolate in this study and the level of contamination present in the cocoa beans, this experiment demonstrated that 93.6% of ochratoxin A present in the beans was reduced during the chocolate producing. Copyright © 2012 Elsevier Ltd. All rights reserved.

  9. Application of gas chromatography to analysis of spirit-based alcoholic beverages.

    Science.gov (United States)

    Wiśniewska, Paulina; Śliwińska, Magdalena; Dymerski, Tomasz; Wardencki, Waldemar; Namieśnik, Jacek

    2015-01-01

    Spirit-based beverages are alcoholic drinks; their production processes are dependent on the type and origin of raw materials. The composition of this complex matrix is difficult to analyze, and scientists commonly choose gas chromatography techniques for this reason. With a wide selection of extraction methods and detectors it is possible to provide qualitative and quantitative analysis for many chemical compounds with various functional groups. This article describes different types of gas chromatography techniques and their most commonly used associated extraction techniques (e.g., LLE, SPME, SPE, SFE, and SBME) and detectors (MS, TOFMS, FID, ECD, NPD, AED, O or EPD). Additionally, brief characteristics of internationally popular spirit-based beverages and application of gas chromatography to the analysis of selected alcoholic drinks are presented.

  10. Investigating the Retention Mechanisms of Liquid Chromatography Using Solid-Phase Extraction Cartridges

    Science.gov (United States)

    O'Donnell, Mary E.; Musial, Beata A.; Bretz, Stacey Lowery; Danielson, Neil D.; Ca, Diep

    2009-01-01

    Liquid chromatography (LC) experiments for the undergraduate analytical laboratory course often illustrate the application of reversed-phase LC to solve a separation problem, but rarely compare LC retention mechanisms. In addition, a high-performance liquid chromatography instrument may be beyond what some small colleges can purchase. Solid-phase…

  11. Instrument platforms for nano liquid chromatography

    Czech Academy of Sciences Publication Activity Database

    Šesták, Jozef; Moravcová, Dana; Kahle, Vladislav

    2015-01-01

    Roč. 1421, NOV (2015), s. 2-17 ISSN 0021-9673 R&D Projects: GA MV VG20112015021 Institutional support: RVO:68081715 Keywords : nano liquid chromatography * splitless gradient generation * nano LC platforms Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 3.926, year: 2015 http://hdl.handle.net/11104/0250900

  12. Bibliography of extraction chromatography, ch. 15

    International Nuclear Information System (INIS)

    Eschrich, H.; Drent, W.

    1975-01-01

    A bibliography of reviews, books and publications dealing with laminar extraction chromatography is given. A tabular survey of experimental data on column extraction chromatographic investigations, stationary phases and support materials is presented. An author index and corporative author index are included. This bibliography refers to various publications relevant to nuclear interest

  13. Enrichment and Determination of radionuclides by ion chromatography

    International Nuclear Information System (INIS)

    ZAFIMANJATO, J.L.R.

    1996-01-01

    The fundamentals of Ion Chromatography (IC) and Liquid Scintillation Counting (LSC) are reviewed. Ion Chromatography as separation method for cations is coupled with Liquid Scintillation Counting for the determination of Radionuclides in water samples. An experimental arrangement for investigations on the applicability of guard columns for cationic radionuclide enrichment is shown. The saturation behaviour of single and bivalentic cations and their combination is presented. Our results show that radioactive bivalentic cations like strontium-90 and radium-226 are enriched on a Ion Pac CG 12 Dionex guard column from 100 to 300ml natural water in one single step. The procedure is suitable for their determination in concentrations down to 10 -2 Bq.l -1 [fr

  14. The effect of SiC particle size on the properties of Cu–SiC composites

    International Nuclear Information System (INIS)

    Celebi Efe, G.; Zeytin, S.; Bindal, C.

    2012-01-01

    Graphical abstract: The relative densities of Cu–SiC composites sintered at 700 °C for 2 h are ranged from 97.3% to 91.8% for SiC with 1 μm particle size and 97.5% to 95.2% for SiC with 5 μm particle size, microhardness of composites ranged from 143 to 167 HV for SiC having 1 μm particle size and 156–182 HVN for SiC having 5 μm particle size and the electrical conductivity of composites changed between 85.9% IACS and 55.7% IACS for SiC with 1 μm particle size, 87.9% IACS and 65.2%IACS for SiC with 5 μm particle size. It was found that electrical conductivity of composites containing SiC with 5 μm particle size is better than that of Cu–SiC composites containing SiC with particle size of 1 μm. Highlights: ► In this research, the effect of SiC particle size on some properties of Cu–SiC composites were investigated. ► The mechanical properties were improved. ► The electrical properties were obtained at desirable level. -- Abstract: SiC particulate-reinforced copper composites were prepared by powder metallurgy (PM) method and conventional atmospheric sintering. Scanning electron microscope (SEM), X-ray diffraction (XRD) techniques were used to characterize the sintered composites. The effect of SiC content and particle size on the relative density, hardness and electrical conductivity of composites were investigated. The relative densities of Cu–SiC composites sintered at 700 °C for 2 h are ranged from 97.3% to 91.8% for SiC with 1 μm particle size and from 97.5% to 95.2% for SiC with 5 μm particle size. Microhardness of composites ranged from 143 to 167 HV for SiC having 1 μm particle size and from 156 to 182 HV for SiC having 5 μm particle size. The electrical conductivity of composites changed between 85.9% IACS and 55.7% IACS for SiC with 1 μm particle size, between 87.9% IACS and 65.2% IACS for SiC with 5 μm particle size.

  15. Potencial de melhoramento e divergência genética de cultivares de milho-pipoca Potential to breeding and genetic divergence in popcorn cultivars

    Directory of Open Access Journals (Sweden)

    Glauco Vieira Miranda

    2003-06-01

    Full Text Available O objetivo deste trabalho foi avaliar o potencial de melhoramento e a divergência genética de nove cultivares tropicais de milho-pipoca. A divergência genética foi estimada por meio da técnica de análise multivariada e as cultivares foram agrupadas com base na distância generalizada de Mahalanobis (DGM, utilizando o método de otimização de Tocher e a dispersão gráfica. Com produtividade de grãos acima de 3 t/ha, destacaram-se as cultivares CMS 43, IAC 112, Viçosa, CMS 42 e Branco, e com índices de capacidade de expansão acima de 24 (v/v, as cultivares IAC 112, RS 20 e Zélia. As estimativas da DGM indicaram (RS 20 e Beija-flor e (Rosa-claro e RS 20 os pares de cultivares mais distantes geneticamente, e (IAC 112 e Viçosa e (Branco e CMS 42, os pares mais similares. Foram identificados três ou quatro grupos divergentes dependendo do método de agrupamento. Para o melhoramento de milho-pipoca, as cultivares com maiores potenciais são RS 20, Zélia, IAC 112 e Beija-flor. As cultivares apresentam divergência genética.The objective of this paper was to evaluate the potential of breeding and genetic divergence in nine tropical popcorn cultivars. The genetic divergence was estimated using multivariate analysis techniques and the cultivars were grouped based in Mahalanobis' generalized distance (MGD, using Tocher's optimization and graphic dispersion. The best cultivars concerning the yield grain above 3 ton/ha were CMS 43, IAC 112, Viçosa, CMS 42 and Branco, and to popping expansion above 24 (v/v were IAC 112, RS 20 and Zélia. The estimates of MGD indicated the pairs genetically more distant (RS 20, Beija-flor and (Rosa-claro, RS 20 as well as pairs genetically more similar (IAC 112, Viçosa and (Branco, CMS 42. Tree or four genetic divergences groups were formed depending on the method. To popcorn breeding, cultivars with best potential are RS 20, Zélia, IAC 112, and Beija-flor. The cultivars show genetic divergence.

  16. Nanomaterials as stationary phases and supports in liquid chromatography.

    Science.gov (United States)

    Beeram, Sandya R; Rodriguez, Elliott; Doddavenkatanna, Suresh; Li, Zhao; Pekarek, Allegra; Peev, Darin; Goerl, Kathryn; Trovato, Gianfranco; Hofmann, Tino; Hage, David S

    2017-10-01

    The development of various nanomaterials over the last few decades has led to many applications for these materials in liquid chromatography (LC). This review will look at the types of nanomaterials that have been incorporated into LC systems and the applications that have been explored for such systems. A number of carbon-based nanomaterials and inorganic nanomaterials have been considered for use in LC, ranging from carbon nanotubes, fullerenes and nanodiamonds to metal nanoparticles and nanostructures based on silica, alumina, zirconia and titanium dioxide. Many ways have been described for incorporating these nanomaterials into LC systems. These methods have included covalent immobilization, adsorption, entrapment, and the synthesis or direct development of nanomaterials as part of a chromatographic support. Nanomaterials have been used in many types of LC. These applications have included the reversed-phase, normal-phase, ion-exchange, and affinity modes of LC, as well as related methods such as chiral separations, ion-pair chromatography and hydrophilic interaction liquid chromatography. Both small and large analytes (e.g., dyes, drugs, amino acids, peptides and proteins) have been used to evaluate possible applications for these nanomaterial-based methods. The use of nanomaterials in columns, capillaries and planar chromatography has been considered as part of these efforts. Potential advantages of nanomaterials in these applications have included their good chemical and physical stabilities, the variety of interactions many nanomaterials can have with analytes, and their unique retention properties in some separation formats. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Strong Cation Exchange Chromatography in Analysis of Posttranslational Modifications: Innovations and Perspectives

    Science.gov (United States)

    Edelmann, Mariola J.

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide. PMID:22174558

  18. UHPLC: The Greening Face of Liquid Chromatography.

    Science.gov (United States)

    Cielecka-Piontek, Judyta; Zalewski, Przemysław; Jelińska, Anna; Garbacki, Piotr

    2013-01-01

    Pharmaceutical analysis based on chromatographic separation is an important part of studies aimed at developing routine quality analysis of drugs. High-performance liquid chromatography (HPLC) is one of the main analytical techniques recommended for drug analysis. Although it meets many criteria vital for analysis, it is time-consuming and uses a relatively high amount of organic solvents compared to other analytical techniques. Recently, Ultra-high-performance liquid chromatography (UHPLC) has been frequently proposed as an alternative to HPLC, which means introducing an environment-friendly approach to drug analysis achieved by reducing the consumption of solvents. It also offers greater chromatographic resolution and higher sensitivity as well as requiring less time due to faster analysis. This review focuses on the basics of UHPLC, compares that technique with HPLC and discusses the possibilities of applying UHPLC for the analysis of different pharmaceuticals and biopharmaceuticals.

  19. Homochiral metal-organic frameworks and their application in chromatography enantioseparations.

    Science.gov (United States)

    Peluso, Paola; Mamane, Victor; Cossu, Sergio

    2014-10-10

    The last frontier in the chiral stationary phases (CSPs) field for chromatography enantioseparations is represented by homochiral metal-organic frameworks (MOFs), a class of organic-inorganic hybrid materials built from metal-connecting nodes and organic-bridging ligands. The modular nature of these materials allows to design focused structures by combining properly metal, organic ligands and rigid polytopic spacers. Intriguingly, chiral ligands introduce molecular chirality in the MOF-network as well as homochirality in the secondary structure of materials (such as homohelicity) producing homochiral nets in a manner mimicking biopolymers (proteins, polysaccharides) which are characterized by a definite helical sense associated with the chirality of their building blocks (amino acids or sugars). Nowadays, robust and flexible materials characterized by high porosity and surface area became available by using preparative procedures typical of the so-called reticular synthesis. This review focuses on recent developments in the synthesis and applications of homochiral MOFs as supports for chromatography enantioseparations. Indeed, despite this field is in its infancy, interesting results have been produced and a critical overview of the 12 reported applications for gas chromatography (GC) and high-performance liquid chromatography (HPLC) can orient the reader approaching the field. Mechanistic aspects are shortly discussed and a view regarding future trends in this field is provided. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Comparative study of radio gas-chromatography and gas chromatography - mass spectrometry coupling in the identification of metabolites of estrogens and progesterone

    International Nuclear Information System (INIS)

    Adessi, G.; Nhuan, T.Q.; Jayle, M.F.

    1978-01-01

    Radio-gas chromatography (RGC) and gas chromatography-mass spectrometry (GC-MS) were used to identify estrogen and progesterone metabolites. The RGC enables the identification of metabolites of labelled precursors ( 3 H)-estradiol-17β and ( 14 C)-progesterone were used as precursors. The GC-MS analytical technique with mass fragmentography, offers the interest of using unlabelled precursors at physiological levels. The identification of metabolites was based on obtaining the mass spectrum or the compiled fragmentogram on the basis of the most characteristic fragment ions. More over, several metabolites can be quantified on the same fragmentogram. Results on the metabolism of estradiol-17β and progesterone by the hepatic tissue of guinea pigs are given. (Auth.)

  1. Proceedings of the DAE-BRNS theme meeting on ion chromatography separations - state of art and perspectives

    International Nuclear Information System (INIS)

    Jeyakumar, S.; Ramakumar, K.L.

    2012-01-01

    Ion Chromatography (IC) plays a vital role in all disciplines of science and technology. In the field of trace separations and speciation studies, use of IC techniques becomes indispensable. In nuclear technology, IC plays a pivotal role in the reactor water chemistry, in the front end of fuel cycle especially in the characterization of nuclear materials including the reactor fuels, post irradiation examination, actinide speciation studies and in understanding the interaction and migration of actinide species in the geo environment. Ion chromatography is also useful in the studies related to waste management particularly for the separation and determination of fission products. The aim of this meeting is to provide a forum to all the researchers in the area of ion chromatography to discuss their recent findings and information, to learn from the mutual experiences and interests, and to promote cooperation both nationally and internationally. Ion chromatography techniques including Ion Chromatography Separations and Nuclear Materials, Speciation Studies by Ion chromatography, Hyphenated -IC Techniques, Reactor Water Chemistry and Ion Chromatography, Solid Phase Extraction and Sample Preparations for IC and Separation of Bio-molecules and Environmental aspects etc are discussed. Papers relevant to INIS are indexed separately

  2. The isotope separation by ion exchange chromatography. Application to the lithium isotopes separation; La separation isotopique par chromatographie ionique

    Energy Technology Data Exchange (ETDEWEB)

    Albert, M G; Barre, Y; Neige, R

    1994-12-31

    In this work is described the used study step to demonstrate the industrial feasibility of a lithium isotopes separation process by ion exchange chromatography. After having recalled how is carried out the exchange reaction between the lithium isotopes bound on the cations exchanger resin and those which are in solution and gave the ion exchange chromatography principle, the authors establish a model which takes into account the cascade theory already used for enriched uranium production. The size parameters of this model are: the isotopic separation factor (which depends for lithium of the ligands nature and of the coordination factor), the isotopic exchange kinetics and the mass flow (which depends of the temperature, the lithium concentration, the resins diameter and the front advance). The way they have to be optimized and the implementation of the industrial process are given. (O.M.). 5 refs.

  3. Microbial metabolomics with gas chromatography/mass spectrometry

    NARCIS (Netherlands)

    Koek, M.M.; Muilwijk, B.; Werf, M.J. van der; Hankemeier, T.

    2006-01-01

    An analytical method was set up suitable for the analysis of microbial metabolomes, consisting of an oximation and silylation derivatization reaction and subsequent analysis by gas chromatography coupled to mass spectrometry. Microbial matrixes contain many compounds that potentially interfere with

  4. Oriented immobilized anti-hIgG via F(c) fragment-imprinted PHEMA cryogel for IgG purification.

    Science.gov (United States)

    Bereli, Nilay; Ertürk, Gizem; Tümer, M Aşkin; Say, Ridvan; Denizli, Adil

    2013-05-01

    Antibodies are used in many applications, especially as diagnostic and therapeutic agents. Among the various techniques used for the purification of antibodies, immunoaffinity chromatography is by far the most common. For this purpose, oriented immobilization of antibodies is an important step for the efficiency of purification step. In this study, F(c) fragment-imprinted poly(hydroxyethyl methacrylate) cryogel (MIP) was prepared for the oriented immobilization of anti-hIgG for IgG purification from human plasma. Non-imprinted poly(hydroxyethyl methacrylate) cryogel (NIP) was also prepared for random immobilization of anti-hIgG to compare the adsorption capacities of oriented (MIP/anti-hIgG) and random (NIP/anti-hIgG) cryogel columns. The amount of immobilized anti-hIgG was 19.8 mg/g for the NIP column and 23.7 mg/g for the MIP column. Although the amount of immobilized anti-hIgG was almost the same for the NIP and MIP columns, IgG adsorption capacity was found to be three times higher than the NIP/anti-hIgG column (29.7 mg/g) for the MIP/anti-hIgG column (86.9 mg/g). Higher IgG adsorption capacity was observed from human plasma (up to 106.4 mg/g) with the MIP/anti-hIgG cryogel column. Adsorbed IgG was eluted using 1.0 M NaCl with a purity of 96.7%. The results obtained here are very encouraging and showed the usability of MIP/anti-hIgG cryogel prepared via imprinting of Fc fragments as an alternative to conventional immunoaffinity techniques for IgG purification. Copyright © 2012 John Wiley & Sons, Ltd.

  5. Alternatives to Chromatography in Plant Breeding

    Directory of Open Access Journals (Sweden)

    Keusgen, Michael

    2016-07-01

    Full Text Available Wild plants were taken into cultivation because of special features. Usually, medicinal plants or spices show distinct secondary metabolites combined with a specific pattern of these compounds. Typically, chromatographic methods like gas chromatography (GC or high performance liquid chromatography (HPLC were applied as standard methods for a meaningful analysis of secondary metabolites. However, these methods are labor and time intensive. In the breeding process, usually numerous single plants have to be analyzed and therefore, high throughput methods are required. In this article, some examples for alternative strategies are given. Besides spectroscopic methods like near infrared (NIR, also biosensoric approaches should be considered. For instance, several enzymes can oxidize or hydrolyze secondary metabolites in dependence of their functional groups. Polyphenols can be determined by laccases. Polyphenols like catechins and flavonoids contribute to the bioactivity of many medicinal plants. Also cysteine sulfoxides, which are typical for Allium species like garlic and onions, can be enzymatically determined with high specificity. Finally, toxic cyanogenic glycosides can be quantified by the enzyme cyanidase.

  6. Bioactive peptides released from Saccharomyces cerevisiae under accelerated autolysis in a wine model system.

    Science.gov (United States)

    Alcaide-Hidalgo, J M; Pueyo, E; Polo, M C; Martínez-Rodríguez, A J

    2007-09-01

    The ACE inhibitory activity (IACE) and the oxygen radical absorbance capacity (ORAC-FL) values of yeast peptides isolated from a model wine during accelerated autolysis of Saccharomyces cerevisiae have been studied. Samples were taken at 6, 24, 48, 121, and 144 h of autolysis. Peptide concentration increased throughout autolysis process. Peptides were fractionated into 2 fractions: F1, constituted by hydrophilic peptides, and F2, containing hydrophobic peptides. Both IACE activity and ORAC-FL values increased during 121 h of autolysis, then decreased afterward. Peptide fraction F2 was the main fraction involved in IACE activity and ORAC-FL.

  7. Use of low volatility mobile phases in electroosmotic thin-layer chromatography.

    Science.gov (United States)

    Berezkin, V G; Balushkin, A O; Tyaglov, B V; Litvin, E F

    2005-08-19

    A variant of electroosmotic thin-layer chromatography is suggested with the use of low volatility compounds as mobile phases aimed at drastically decreasing the evaporation of the mobile phase and improving the reproducibility of the method. The linear movement velocity of zones of separated compounds is experimentally shown to increase 2-12-fold in electroosmotic chromatography (compared to similar values in traditional TLC). The separation efficiency is also considerably increased.

  8. Monodisperse microbeads of hypercrosslinked polystyrene for liquid and supercritical fluid chromatography

    Science.gov (United States)

    Tsyurupa, M. P.; Blinnikova, Z. K.; Il'in, M. M.; Davankov, V. A.; Parenago, O. O.; Pokrovskii, O. I.; Usovich, O. I.

    2015-11-01

    Monodisperse styrene-divinylbenzene (1 wt %) copolymer microbeads are obtained via the elaborate method of high-productivity precipitation polymerization. The crosslinking of this copolymer with chloromethyl methyl ether in the presence of Friedel-Crafts catalyst yields porous hypercrosslinked polymers with degrees of crosslinking that range from 200 to 500%. Microbead sorbents are shown to be suited for selective stationary phases for high-performance liquid chromatography and supercritical fluid chromatography.

  9. Forensic applications of supercritical fluid chromatography - mass spectrometry.

    Science.gov (United States)

    Pauk, Volodymyr; Lemr, Karel

    2018-06-01

    Achievements of supercritical fluid chromatography with mass spectrometric detection made in the field of forensic science during the last decade are reviewed. The main topics include analysis of traditional drugs of abuse (e.g. cannabis, methamphetamine) as well as new psychoactive substances (synthetic cannabinoids, cathinones and phenethylamines), doping agents (anabolic steroids, stimulants, diuretics, analgesics etc.) and chemical warfare agents. Control of food authenticity, detection of adulteration and identification of toxic substances in food are also pointed out. Main aspects of an analytical workflow, such as sample preparation, separation and detection are discussed. A special attention is paid to the performance characteristics and validation parameters of supercritical fluid chromatography-mass spectrometric methods in comparison with other separation techniques. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Baseline and follow-up MRI of the internal auditory canal after suboccipital resection of acoustic schwannoma: appearances and clinical correlations

    International Nuclear Information System (INIS)

    Smith, M.; Castillo, M.; Campbell, J.; Pillsbury, H.; Walters, T.

    1995-01-01

    Prospective baseline MRI was obtained on 31 patients who had ''total'' removal of acoustic schwannoma 6 months to 9 years previously. Follow-up MRI was performed after 1-2 years on patients with questionable abnormalities. We found four patterns (1) internal auditory canals (IAC) with nonenhancing soft-tissue strands, possibly scars or distorted residual nerves (8); (2) IAC with marginal enhancement-reactive dura mater (16); (3) IAC with contrast-enhancing globular tissues suggesting residual or recurrent tumour (5); (4) high-signal intensity in the IAC before contrast medium administration, probably related to graft with fat/fascia/muscle (2). Prospective 1- to 2-year follow-up studies were available in 8, 5, and 1 patients in groups 2, 3, and 4 respectively. In group 2, dural enhancement remained unchanged in 5 patients and decreased in 3. In group 3 follow-up showed 1 tumor recurrence (surgically confirmed) and 4 stable abnormalities. In group 4, follow-up in 1 of the 2 patients was stable. In groups 1 and 2, the MRI features correlate well with complete tumor removal. Whether follow-up in these groups is indicated needs to be determined. In group 3 residual or recurrent tumor cannot be excluded. In group 4, grafts may prevent adequate visualization of the IAC. (orig.)

  11. The cochlear nerve canal and internal auditory canal in children with normal cochlea but cochlear nerve deficiency

    International Nuclear Information System (INIS)

    Yan, Fei; Li, Jianhong; Xian, Junfang; Wang, Zhenchang; Mo, Lingyan

    2013-01-01

    Background: There is an increasing frequency of requests for cochlear implantation (CI) in deaf children and more detailed image information is necessary for selecting appropriate candidates. Cochlear nerve deficiency (CND) is a contraindication to CI. Magnetic resonance imaging (MRI) has been used to evaluate the integrity of the cochlear nerve. The abnormalities of the cochlear nerve canal (CNC) and internal auditory canal (IAC) have been reported to be associated with CND. Purpose: To correlate CNC manifestation, size, and IAC diameter on high-resolution CT (HRCT) with CND diagnosed by MRI in children. Material and Methods: HRCT images from 35 sensorineurally deaf children who had normal cochlea but bilateral or unilateral CND diagnosed by MRI were studied retrospectively. The CNC and IAC manifestation and size were assessed and correlated with CND. Results: CND was diagnosed by MRI in 54/70 ears (77.1%). Thirty-two ears had an absent cochlear nerve (59.3%), while 22 ears had a small cochlear nerve (40.7%). The CNC diameter was 2.0 mm in 11 ears (20.4%). The IAC diameter was 3.0 mm in 29 ears (53.7%). Conclusion: The hypoplastic CNC might be more highly indicative of CND than that of a narrow IAC

  12. Intra-arterial chemotherapy combined with irradiation for invasive bladder cancer

    International Nuclear Information System (INIS)

    Fujimoto, Naohiro; Sato, Hideki; Harada, Shuji; Matsumoto, Tetsuro; Ikuyama, Toshihiro

    2004-01-01

    Total cystectomy and urinary diversion are the standard treatments for invasive bladder cancer. However, total cystectomy is not possible in some patients due to advanced age, a poor general condition, or refusal to undergo cystectomy. In such cases, intra-arterial chemotherapy (IAC) and/or radiotherapy are the alternative treatments. We performed IAC with cisplatin and adriamycin in 9 patients with invasive bladder cancer and obtained complete response (CR) in 5 out of the 9 patients (55.6%). However, 3 of these 5 CR patients developed local recurrence within 1 year. In an effort to improve the efficacy, we performed combination therapy comprising IAC plus radiotherapy in 12 patients with invasive bladder cancer. CR was obtained in 58.3% and the bladder was preserved in 91.7% with this combination therapy. However, distant metastases developed in 33.3% after the combined treatment of IAC plus radiation therapy. These findings suggest that the combination of radiotherapy and IAC is useful for local control of invasive bladder cancer. Data from more cases and results from a longer follow-up are needed to fully confirm the efficacy of this type of treatment. In addition, therapeutic modalities to prevent distant metastasis need to be considered. (author)

  13. Instrumentation for analytical scale supercritical fluid chromatography.

    Science.gov (United States)

    Berger, Terry A

    2015-11-20

    Analytical scale supercritical fluid chromatography (SFC) is largely a sub-discipline of high performance liquid chromatography (HPLC), in that most of the hardware and software can be used for either technique. The aspects that separate the 2 techniques stem from the use of carbon dioxide (CO2) as the main component of the mobile phase in SFC. The high compressibility and low viscosity of CO2 mean that pumps, and autosamplers designed for HPLC either need to be modified or an alternate means of dealing with compressibility needs to be found. The inclusion of a back pressure regulator and a high pressure flow cell for any UV-Vis detector are also necessary. Details of the various approaches, problems and solutions are described. Characteristics, such as adiabatic vs. isothermal compressibility, thermal gradients, and refractive index issues are dealt with in detail. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. Produtividade e qualidade dos frutos da laranjeira 'Pêra' clone IAC em 16 porta-enxertos na região de Bebedouro-SP Yield and fruit quality of 'Pêra' sweet orange clone IAC on 16 rootstocks in Bebedouro region, State of São Paulo, Brazil

    Directory of Open Access Journals (Sweden)

    Eduardo Sanches Stuchi

    2004-08-01

    and chemical fruit characteristics such as fruit size, total soluble solids, acidity, ratio juice content and technological index of 'Pera' IAC sweet orange [Citrus sinensis (L. Osbeck], in a high inoculum pressure area of citrus variegated chlorosis (CVC. The spacement was 6.0 m between rows and 3.5 m between trees. The experimental design used was randomized blocks, with three replications and two trees per plot. The rootstocks tested were 'Sun Chu Sha Kat' mandarin (Citrus reticulata, 'Pectinífera' (C. reticulata, 'Shekwasha' (C. depressa Hayata, 'Pectinífera/Shekwasha' (C. depressa Hayata, 'Batangas' (C. reticulata, 'Oneco' (C. reticulata, citrangor [citrange (Poncirus trifoliata Raf. x C. sinensis x C. sinensis], citrandarin (C. sunki hort. ex Tanaka x Poncirus trifoliata L. Raf. cv. English, 'Sunki' (C. sunki, 'Suen-Kat' (C. sunki, Nasnaran (C. amblycarpa Ochse, 'Venezuela' mandarin (C. reticulata, 'Heen Naran' mandarin (C. lycopersicaeformis, 'Cravo' (C. limonia Osbeck x 'Cleopatra' (C. reshni hort ex Tanaka, 'Cravo' (C. limonia, 'Cleopatra' (C. reshni. CVC intensity was different due to rootstocks effects and not related with yield until the fourth year of production. With the exception of the Nasnaran mandarin the rootstocks induced initial fruit production and quality similar to 'Cravo'.

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

    Science.gov (United States)

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

    2017-09-15

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

  16. Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

    Science.gov (United States)

    Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

    2016-02-01

    A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

  17. Investigating interactions between phospholipase B-Like 2 and antibodies during Protein A chromatography.

    Science.gov (United States)

    Tran, Benjamin; Grosskopf, Vanessa; Wang, Xiangdan; Yang, Jihong; Walker, Don; Yu, Christopher; McDonald, Paul

    2016-03-18

    Purification processes for therapeutic antibodies typically exploit multiple and orthogonal chromatography steps in order to remove impurities, such as host-cell proteins. While the majority of host-cell proteins are cleared through purification processes, individual host-cell proteins such as Phospholipase B-like 2 (PLBL2) are more challenging to remove and can persist into the final purification pool even after multiple chromatography steps. With packed-bed chromatography runs using host-cell protein ELISAs and mass spectrometry analysis, we demonstrated that different therapeutic antibodies interact to varying degrees with host-cell proteins in general, and PLBL2 specifically. We then used a high-throughput Protein A chromatography method to further examine the interaction between our antibodies and PLBL2. Our results showed that the co-elution of PLBL2 during Protein A chromatography is highly dependent on the individual antibody and PLBL2 concentration in the chromatographic load. Process parameters such as antibody resin load density and pre-elution wash conditions also influence the levels of PLBL2 in the Protein A eluate. Furthermore, using surface plasmon resonance, we demonstrated that there is a preference for PLBL2 to interact with IgG4 subclass antibodies compared to IgG1 antibodies. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. Use of laminar chromatographic methods for determination of separation conditions in column extraction chromatography

    International Nuclear Information System (INIS)

    Ghersini, G.; Cerrai, E.

    1978-01-01

    Possibilities of using laminar chromatographic methods (paper and thin-layer chromatography) to determine optimal separation conditions in column extraction chromatography are analysed. Most of the given laminar methods are presented as Rf-spectra, i.e. as dependences of Rf found experimentally on eluating solution component concentration. Interrelation between Rf and distribution coefficients of corresponding liquid extraction systems and retention volumes of chromatographic columns is considered. Literature data on extraction paper and thin-layer chromatography of elements with various immovable phases are presented

  19. Isolation of oxidative degradation products of atorvastatin with supercritical fluid chromatography.

    Science.gov (United States)

    Klobčar, Slavko; Prosen, Helena

    2015-12-01

    The isolation of four oxidative degradation products of atorvastatin using preparative high-performance liquid chromatography applying at least two chromatographic steps is known from the literature. In this paper it is shown that the same four impurities could be isolated from similarly prepared mixtures in only one step using supercritical fluid chromatography. The methods for separation were developed and optimized. The preparation of the mixtures was altered in such a way as to enhance the concentration of desired impurities. Appropriate solvents were applied for collection of separated impurities in order to prevent degradation. The structures of the isolated impurities were confirmed and their purity determined. The preparative supercritical fluid chromatography has proven to be superior to preparative HPLC regarding achieved purity of standards applying fewer chromatographic as well as isolation steps. Copyright © 2015 John Wiley & Sons, Ltd.

  20. Recent advances in liquid and gas chromatography methodology for extending coverage of the metabolome.

    Science.gov (United States)

    Haggarty, Jennifer; Burgess, Karl Ev

    2017-02-01

    The metabolome is the complete complement of metabolites (small organic biomolecules). In order to comprehensively understand the effect of stimuli on a biological system, it is important to detect as many of the metabolites within that system as possible. This review briefly describes some new advances in liquid and gas chromatography to improve coverage of the metabolome, including the serial combination of two columns in tandem, column switching and different variations of two-dimensional chromatography. Supercritical fluid chromatography could provide complimentary data to liquid and gas chromatography. Although there have been many recent advancements in the field of metabolomics, it is evident that a combination, rather than a single method, is required to approach full coverage of the metabolome. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.