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Sample records for biologically unrealistic sampling

  1. What is unrealistic optimism?

    Science.gov (United States)

    Jefferson, Anneli; Bortolotti, Lisa; Kuzmanovic, Bojana

    2017-04-01

    Here we consider the nature of unrealistic optimism and other related positive illusions. We are interested in whether cognitive states that are unrealistically optimistic are belief states, whether they are false, and whether they are epistemically irrational. We also ask to what extent unrealistically optimistic cognitive states are fixed. Based on the classic and recent empirical literature on unrealistic optimism, we offer some preliminary answers to these questions, thereby laying the foundations for answering further questions about unrealistic optimism, such as whether it has biological, psychological, or epistemic benefits. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

  2. What is unrealistic optimism?

    OpenAIRE

    Jefferson, Anneli; Bortolotti, Lisa; Kuzmanovic, Bojana

    2017-01-01

    Here we consider the nature of unrealistic optimism and other related positive illusions. We are interested in whether cognitive states that are unrealistically optimistic are belief states, whether they are false, and whether they are epistemically irrational. We also ask to what extent unrealistically optimistic cognitive states are fixed. Based on the classic and recent empirical literature on unrealistic optimism, we offer some preliminary answers to these questions, thereby laying the fo...

  3. Taking Stock of Unrealistic Optimism.

    Science.gov (United States)

    Shepperd, James A; Klein, William M P; Waters, Erika A; Weinstein, Neil D

    2013-07-01

    Researchers have used terms such as unrealistic optimism and optimistic bias to refer to concepts that are similar but not synonymous. Drawing from three decades of research, we critically discuss how researchers define unrealistic optimism and we identify four types that reflect different measurement approaches: unrealistic absolute optimism at the individual and group level and unrealistic comparative optimism at the individual and group level. In addition, we discuss methodological criticisms leveled against research on unrealistic optimism and note that the criticisms are primarily relevant to only one type-the group form of unrealistic comparative optimism. We further clarify how the criticisms are not nearly as problematic even for unrealistic comparative optimism as they might seem. Finally, we note boundary conditions on the different types of unrealistic optimism and reflect on five broad questions that deserve further attention.

  4. Taking Stock of Unrealistic Optimism

    Science.gov (United States)

    Shepperd, James A.; Klein, William M. P.; Waters, Erika A.; Weinstein, Neil D.

    2015-01-01

    Researchers have used terms such as unrealistic optimism and optimistic bias to refer to concepts that are similar but not synonymous. Drawing from three decades of research, we critically discuss how researchers define unrealistic optimism and we identify four types that reflect different measurement approaches: unrealistic absolute optimism at the individual and group level and unrealistic comparative optimism at the individual and group level. In addition, we discuss methodological criticisms leveled against research on unrealistic optimism and note that the criticisms are primarily relevant to only one type—the group form of unrealistic comparative optimism. We further clarify how the criticisms are not nearly as problematic even for unrealistic comparative optimism as they might seem. Finally, we note boundary conditions on the different types of unrealistic optimism and reflect on five broad questions that deserve further attention. PMID:26045714

  5. Biological sample collector

    Science.gov (United States)

    Murphy, Gloria A [French Camp, CA

    2010-09-07

    A biological sample collector is adapted to a collect several biological samples in a plurality of filter wells. A biological sample collector may comprise a manifold plate for mounting a filter plate thereon, the filter plate having a plurality of filter wells therein; a hollow slider for engaging and positioning a tube that slides therethrough; and a slide case within which the hollow slider travels to allow the tube to be aligned with a selected filter well of the plurality of filter wells, wherein when the tube is aligned with the selected filter well, the tube is pushed through the hollow slider and into the selected filter well to sealingly engage the selected filter well and to allow the tube to deposit a biological sample onto a filter in the bottom of the selected filter well. The biological sample collector may be portable.

  6. Unrealistic Optimism: East and West?

    Science.gov (United States)

    Joshi, Mary Sissons; Carter, Wakefield

    2013-01-01

    Following Weinstein’s (1980) pioneering work many studies established that people have an optimistic bias concerning future life events. At first, the bulk of research was conducted using populations in North America and Northern Europe, the optimistic bias was thought of as universal, and little attention was paid to cultural context. However, construing unrealistic optimism as a form of self-enhancement, some researchers noted that it was far less common in East Asian cultures. The current study extends enquiry to a different non-Western culture. Two hundred and eighty seven middle aged and middle income participants (200 in India, 87 in England) rated 11 positive and 11 negative events in terms of the chances of each event occurring in “their own life,” and the chances of each event occurring in the lives of “people like them.” Comparative optimism was shown for bad events, with Indian participants showing higher levels of optimism than English participants. The position regarding comparative optimism for good events was more complex. In India those of higher socioeconomic status (SES) were optimistic, while those of lower SES were on average pessimistic. Overall, English participants showed neither optimism nor pessimism for good events. The results, whose clinical relevance is discussed, suggest that the expression of unrealistic optimism is shaped by an interplay of culture and socioeconomic circumstance. PMID:23407689

  7. Enhanced Biological Sampling Data

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — This is a database of a variety of biological, reproductive, and energetic data collected from fish on the continental shelf in the northwest Atlantic Ocean. Species...

  8. Biological Sampling Variability Study

    Energy Technology Data Exchange (ETDEWEB)

    Amidan, Brett G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hutchison, Janine R. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-11-08

    There are many sources of variability that exist in the sample collection and analysis process. This paper addresses many, but not all, sources of variability. The main focus of this paper was to better understand and estimate variability due to differences between samplers. Variability between days was also studied, as well as random variability within each sampler. Experiments were performed using multiple surface materials (ceramic and stainless steel), multiple contaminant concentrations (10 spores and 100 spores), and with and without the presence of interfering material. All testing was done with sponge sticks using 10-inch by 10-inch coupons. Bacillus atrophaeus was used as the BA surrogate. Spores were deposited using wet deposition. Grime was coated on the coupons which were planned to include the interfering material (Section 3.3). Samples were prepared and analyzed at PNNL using CDC protocol (Section 3.4) and then cultured and counted. Five samplers were trained so that samples were taken using the same protocol. Each sampler randomly sampled eight coupons each day, four coupons with 10 spores deposited and four coupons with 100 spores deposited. Each day consisted of one material being tested. The clean samples (no interfering materials) were run first, followed by the dirty samples (coated with interfering material). There was a significant difference in recovery efficiency between the coupons with 10 spores deposited (mean of 48.9%) and those with 100 spores deposited (mean of 59.8%). There was no general significant difference between the clean and dirty (containing interfering material) coupons or between the two surface materials; however, there was a significant interaction between concentration amount and presence of interfering material. The recovery efficiency was close to the same for coupons with 10 spores deposited, but for the coupons with 100 spores deposited, the recovery efficiency for the dirty samples was significantly larger (65

  9. Biological Sample Monitoring Database (BSMDBS)

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — The Biological Sample Monitoring Database System (BSMDBS) was developed for the Northeast Fisheries Regional Office and Science Center (NER/NEFSC) to record and...

  10. Microholographic imaging of biological samples

    International Nuclear Information System (INIS)

    Haddad, W.S.; Cullen, D.; Solem, J.C.; Longworth, J.W.; McPherson, A.; Boyer, K.; Rhodes, C.K.

    1990-01-01

    A camera system suitable for x-ray microholography has been constructed. Visible light Fourier transform microholograms of biological samples and other test targets have been recorded and reconstructed digitally using a glycerol microdrop as a reference wave source. Current results give a resolution of ∼4 - 10 λ with λ = 514.5 nm. 11 refs., 1 fig

  11. Electron holography of biological samples.

    Science.gov (United States)

    Simon, P; Lichte, H; Formanek, P; Lehmann, M; Huhle, R; Carrillo-Cabrera, W; Harscher, A; Ehrlich, H

    2008-01-01

    In this paper, we summarise the development of off-axis electron holography on biological samples starting in 1986 with the first results on ferritin from the group of Tonomura. In the middle of the 1990s strong interest was evoked, but then stagnation took place because the results obtained at that stage did not reach the contrast and the resolution achieved by conventional electron microscopy. To date, there exist only a few ( approximately 12) publications on electron holography of biological objects, thus this topic is quite small and concise. The reason for this could be that holography is mostly established in materials science by physicists. Therefore, applications for off-axis holography were powerfully pushed forward in the area of imaging, e.g. electric or magnetic micro- and nanofields. Unstained biological systems investigated by means of off-axis electron holography up to now are ferritin, tobacco mosaic virus, a bacterial flagellum, T5 bacteriophage virus, hexagonal packed intermediate layer of bacteria and the Semliki Forest virus. New results of the authors on collagen fibres and surface layer of bacteria, the so-called S-layer 2D crystal lattice are presented in this review. For the sake of completeness, we will shortly discuss in-line holography of biological samples and off-axis holography of materials related to biological systems, such as biomaterial composites or magnetotactic bacteria.

  12. Assessing the consequences of unrealistic optimism: Challenges and recommendations.

    Science.gov (United States)

    Shepperd, James A; Pogge, Gabrielle; Howell, Jennifer L

    2017-04-01

    Of the hundreds of studies published on unrealistic optimism (i.e., expecting a better personal future than is reasonably likely), most have focused on demonstrating the phenomenon, examining boundary conditions, or documenting causes. Few studies have examined the consequences of unrealistic optimism. In this article, we provide an overview of the measurement of unrealistic optimism, review possible consequences, and identify numerous challenges confronting investigators attempting to understand the consequences. Assessing the consequences of unrealistic optimism is tricky, and ultimately probably impossible when researchers assess unrealistic optimism at the group level (which reveals if a group of people is displaying unrealistic optimism on average) rather than the individual level (which reveals whether a specific individual displays unrealistic optimism). We offer recommendations to researchers who wish to examine the consequences of unrealistic optimism. Copyright © 2016 Elsevier Inc. All rights reserved.

  13. Unrealistic Optimism: Self-Enhancement or Person Positivity?

    Science.gov (United States)

    Regan, Pamela C.; And Others

    1995-01-01

    Two studies examined whether people are unrealistically optimistic only for their own futures or for the future of any individual. Results suggested that unrealistic optimism is a form of self-enhancement rather than person positivity bias. (JBJ)

  14. Biological Environmental Sampling Technologies Assessment

    Science.gov (United States)

    2015-12-01

    assay performance for the detection of target pathogens or protein biomarkers in liquid matrices. The nanomanipulation technology provides a dramatic...personal protective equipment qPCR quantitative polymerase chain reaction RAID Rapid Assessment Initial Detection kit RFI request for information RT...Carrie Poore Robert Dorsey RESEARCH AND TECHNOLOGY DIRECTORATE Aaron Chonko David Grieco JOINT BIOLOGICAL TACTICAL DETECTION SYSTEM

  15. Gallium determination in biological samples

    International Nuclear Information System (INIS)

    Stulzaft, O.; Maziere, B.; Ly, S.

    1980-01-01

    A sensitive, simple and time-saving method has been developed for the neutron activation analysis of gallium at concentrations around 10 -4 ppm in biological tissues. After a 24-hour irradiation in a thermal neutron flux of 2.8x10 13 nxcm -2 xs -1 and a purification by ion-exchange chromatography to eliminate troublesome elements such as sodium, iron and copper, the 72 Ga activity is measured with enough accuracy for the method to be applicable in animal physiology and clinical toxicology. (author)

  16. An improved ashing procedure for biologic sample

    International Nuclear Information System (INIS)

    Wu Zongmei

    1992-01-01

    The classical ashing procedure in muffle was modified for biologic samples. In the modified procedure the door of muffle was open in the duration of ashing process, the ashing was accelerated and the ashing product quality was comparable to that the classical procedure. The modified procedure is suitable for ashing biologic samples in large batches

  17. Sample preparation in biological mass spectrometry

    CERN Document Server

    Ivanov, Alexander R

    2011-01-01

    The aim of this book is to provide the researcher with important sample preparation strategies in a wide variety of analyte molecules, specimens, methods, and biological applications requiring mass spectrometric analysis as a detection end-point.

  18. Determination of thallium in biological samples.

    Science.gov (United States)

    Das, Arabinda K; Chakraborty, Ruma; Cervera, M Luisa; de la Guardia, Miguel

    2006-06-01

    Determination of thallium has become a major interest because of its high toxicity, especially as the monovalent cation. Thallium poisoning in the human body must be checked quickly by analysis of biological samples. This review highlights the development of highly sensitive detection techniques applied to the determination of thallium in biological samples, with or without pretreatment, based on the literature compiled in Analytical Abstracts from 1990.

  19. Modular microfluidic system for biological sample preparation

    Science.gov (United States)

    Rose, Klint A.; Mariella, Jr., Raymond P.; Bailey, Christopher G.; Ness, Kevin Dean

    2015-09-29

    A reconfigurable modular microfluidic system for preparation of a biological sample including a series of reconfigurable modules for automated sample preparation adapted to selectively include a) a microfluidic acoustic focusing filter module, b) a dielectrophoresis bacteria filter module, c) a dielectrophoresis virus filter module, d) an isotachophoresis nucleic acid filter module, e) a lyses module, and f) an isotachophoresis-based nucleic acid filter.

  20. Discovering biological progression underlying microarray samples.

    Directory of Open Access Journals (Sweden)

    Peng Qiu

    2011-04-01

    Full Text Available In biological systems that undergo processes such as differentiation, a clear concept of progression exists. We present a novel computational approach, called Sample Progression Discovery (SPD, to discover patterns of biological progression underlying microarray gene expression data. SPD assumes that individual samples of a microarray dataset are related by an unknown biological process (i.e., differentiation, development, cell cycle, disease progression, and that each sample represents one unknown point along the progression of that process. SPD aims to organize the samples in a manner that reveals the underlying progression and to simultaneously identify subsets of genes that are responsible for that progression. We demonstrate the performance of SPD on a variety of microarray datasets that were generated by sampling a biological process at different points along its progression, without providing SPD any information of the underlying process. When applied to a cell cycle time series microarray dataset, SPD was not provided any prior knowledge of samples' time order or of which genes are cell-cycle regulated, yet SPD recovered the correct time order and identified many genes that have been associated with the cell cycle. When applied to B-cell differentiation data, SPD recovered the correct order of stages of normal B-cell differentiation and the linkage between preB-ALL tumor cells with their cell origin preB. When applied to mouse embryonic stem cell differentiation data, SPD uncovered a landscape of ESC differentiation into various lineages and genes that represent both generic and lineage specific processes. When applied to a prostate cancer microarray dataset, SPD identified gene modules that reflect a progression consistent with disease stages. SPD may be best viewed as a novel tool for synthesizing biological hypotheses because it provides a likely biological progression underlying a microarray dataset and, perhaps more importantly, the

  1. Irradiation chamber and sample changer for biological samples

    International Nuclear Information System (INIS)

    Kraft, G.; Daues, H.W.; Fischer, B.; Kopf, U.; Liebold, H.P.; Quis, D.; Stelzer, H.; Kiefer, J.; Schoepfer, F.; Schneider, E.

    1980-01-01

    This paper describes an irradiaton system with which living cells of different origin are irradiated with heavy ion beams (18 <- Z <- 92) at energies up to 10 MeV/amu. The system consists of a beam monitor connected to the vacuum system of the accelerator and the irradiation chamber, containing the biological samples under atmospheric pressure. The requirements and aims of the set up are discussed. The first results with saccharomyces cerevisiae and Chinese Hamster tissue cells are presented. (orig.)

  2. [The ethical implications of conserving biological samples].

    Science.gov (United States)

    Tazzite, A; Roky, R; Avard, D

    2009-09-01

    The conservation and use of biological samples become more and more frequent all around the world. Biobanks of human body substances (blood, urine, DNA, tissues, cells, etc.), and personal data associated with them are created. They have a double character as they are collections of both human biological samples and personal data. In some cases, the gametes, reproductive tissues, embryos, foetal tissue after abortion or even specimens of dead donors are collected and conserved. Although biobanks raise hopes in both the development of new therapies, new drugs and their integration into clinical medicine, they also point to concerns related to ethical questions such as: the principles of information, the consent of the persons concerned, the confidentiality about the personal data, and in some cases discrimination and stigmatisation. Other ethical aspects could raise gradually as research advance. Research being carried out on human sample requires informed free consent from the person who should be able to consent. The donor must be sufficiently informed about the process of research, the purpose, benefits and the risks involved in participating in this research. In the case of persons unable to give consent such minors or persons with mental disabilities, special measures are undertaken. Once the consent was given, the right of withdrawal has been consistently supported by the various declarations and regulations, but some oppose this right for a number of reasons particularly in the case of research on the samples without risk of physical exposure. In this case the notion of human body integrity is different than in research involving therapeutic or clinical intervention. In the case of withdrawal of consent, the samples should be destroyed, but the anonymous results arising from them and their analysis are not affected. What is the case for future uses? Should the researcher obtain again the consent from the donor for a secondary use of the samples? This is a

  3. PIXE and its applications to biological samples

    International Nuclear Information System (INIS)

    Aldape, F.; Flores, M.J.

    1996-01-01

    Throughout this century, industrialized society has seriously affected the ecology by introducing huge amounts of pollutants into the atmosphere as well as marine and soil environments. On the other hand, it is known that these pollutants, in excess of certain levels of concentration, not only put at risk the life of living beings but may also cause the extinction of some species. It is therefore of basic importance to substantially increase quantitative determinations of trace element concentrations in biological specimens in order to assess the effects of pollutants. It is in this field that PIXE plays a key role in these studies, where its unique analytical properties are decisive. Moreover, since the importance of these research has been recognized in many countries, many scientists have been encouraged to continue or initiate new research programmes aimed to solve the worldwide pollution problem. This document presents an overview of those papers reporting the application of PIXE analysis to biological samples during this last decade of the 20th century and recounts the number of PIXE laboratories dedicating their efforts to find the clues of the biological effects of the presence of pollutants introduced in living beings. Sample preparation methods, different kinds of samples under study and the use of complementary analytical techniques are also illustrated. (author). 108 refs

  4. Accelerator mass spectrometry of small biological samples.

    Science.gov (United States)

    Salehpour, Mehran; Forsgard, Niklas; Possnert, Göran

    2008-12-01

    Accelerator mass spectrometry (AMS) is an ultra-sensitive technique for isotopic ratio measurements. In the biomedical field, AMS can be used to measure femtomolar concentrations of labeled drugs in body fluids, with direct applications in early drug development such as Microdosing. Likewise, the regenerative properties of cells which are of fundamental significance in stem-cell research can be determined with an accuracy of a few years by AMS analysis of human DNA. However, AMS nominally requires about 1 mg of carbon per sample which is not always available when dealing with specific body substances such as localized, organ-specific DNA samples. Consequently, it is of analytical interest to develop methods for the routine analysis of small samples in the range of a few tens of microg. We have used a 5 MV Pelletron tandem accelerator to study small biological samples using AMS. Different methods are presented and compared. A (12)C-carrier sample preparation method is described which is potentially more sensitive and less susceptible to contamination than the standard procedures.

  5. Speciation of arsenic in biological samples.

    Science.gov (United States)

    Mandal, Badal Kumar; Ogra, Yasumitsu; Anzai, Kazunori; Suzuki, Kazuo T

    2004-08-01

    Speciation of arsenicals in biological samples is an essential tool to gain insight into its distribution in tissues and its species-specific toxicity to target organs. Biological samples (urine, hair, fingernail) examined in the present study were collected from 41 people of West Bengal, India, who were drinking arsenic (As)-contaminated water, whereas 25 blood and urine samples were collected from a population who stopped drinking As contaminated water 2 years before the blood collection. Speciation of arsenicals in urine, water-methanol extract of freeze-dried red blood cells (RBCs), trichloroacetic acid treated plasma, and water extract of hair and fingernail was carried out by high-performance liquid chromatography (HPLC)-inductively coupled argon plasma mass spectrometry (ICP MS). Urine contained arsenobetaine (AsB, 1.0%), arsenite (iAs(III), 11.3), arsenate (iAs(V), 10.1), monomethylarsonous acid (MMA(III), 6.6), monomethylarsonic acid (MMA(V), 10.5), dimethylarsinous acid (DMA(III), 13.0), and dimethylarsinic acid (DMA(V), 47.5); fingernail contained iAs(III) (62.4%), iAs(V) (20.2), MMA(V) (5.7), DMA(III) (8.9), and DMA(V) (2.8); hair contained iAs(III) (58.9%), iAs(V) (34.8), MMA(V) (2.9), and DMA(V) (3.4); RBCs contained AsB (22.5%) and DMA(V) (77.5); and blood plasma contained AsB (16.7%), iAs(III) (21.1), MMA(V) (27.1), and DMA(V) (35.1). MMA(III), DMA(III), and iAs(V) were not found in any plasma and RBCs samples, but urine contained all of them. Arsenic in urine, fingernails, and hair are positively correlated with water As, suggesting that any of these measurements could be considered as a biomarker to As exposure. Status of urine and exogenous contamination of hair urgently need speciation of As in these samples, but speciation of As in nail is related to its total As (tAs) concentration. Therefore, total As concentrations of nails could be considered as biomarker to As exposure in the endemic areas.

  6. Speciation of arsenic in biological samples

    International Nuclear Information System (INIS)

    Mandal, Badal Kumar; Ogra, Yasumitsu; Anzai, Kazunori; Suzuki, Kazuo T.

    2004-01-01

    Speciation of arsenicals in biological samples is an essential tool to gain insight into its distribution in tissues and its species-specific toxicity to target organs. Biological samples (urine, hair, fingernail) examined in the present study were collected from 41 people of West Bengal, India, who were drinking arsenic (As)-contaminated water, whereas 25 blood and urine samples were collected from a population who stopped drinking As contaminated water 2 years before the blood collection. Speciation of arsenicals in urine, water-methanol extract of freeze-dried red blood cells (RBCs), trichloroacetic acid treated plasma, and water extract of hair and fingernail was carried out by high-performance liquid chromatography (HPLC)-inductively coupled argon plasma mass spectrometry (ICP MS). Urine contained arsenobetaine (AsB, 1.0%), arsenite (iAs III , 11.3), arsenate (iAs V , 10.1), monomethylarsonous acid (MMA III , 6.6), monomethylarsonic acid (MMA V , 10.5), dimethylarsinous acid (DMA III , 13.0), and dimethylarsinic acid (DMA V , 47.5); fingernail contained iAs III (62.4%), iAs V (20.2), MMA V (5.7), DMA III (8.9), and DMA V (2.8); hair contained iAs III (58.9%), iAs V (34.8), MMA V (2.9), and DMA V (3.4); RBCs contained AsB (22.5%) and DMA V (77.5); and blood plasma contained AsB (16.7%), iAs III (21.1), MMA V (27.1), and DMA V (35.1). MMA III , DMA III , and iAs V were not found in any plasma and RBCs samples, but urine contained all of them. Arsenic in urine, fingernails, and hair are positively correlated with water As, suggesting that any of these measurements could be considered as a biomarker to As exposure. Status of urine and exogenous contamination of hair urgently need speciation of As in these samples, but speciation of As in nail is related to its total As (tAs) concentration. Therefore, total As concentrations of nails could be considered as biomarker to As exposure in the endemic areas

  7. Assessing Biological Samples with Scanning Probes

    Science.gov (United States)

    Engel, A.

    Scanning probe microscopes raster-scan an atomic scale sensor across an object. The scanning transmission electron microscope (STEM) uses an electron beam focused on a few Å, and measures the electron scattering power of the irradiated column of sample matter. Not only does the STEM create dark-filed images of superb clarity, but it also delivers the mass of single protein complexes within a range of 100 kDa to 100 MDa. The STEM appears to be the tool of choice to achieve high-throughput visual proteomics of single cells. In contrast, atomically sharp tips sample the object surface in the scanning tunneling microscope as well as the atomic force microscopes (AFM). Because the AFM can be operated on samples submerged in a physiological salt solution, biomacromolecules can be observed at work. Recent experiments provided new insights into the organization of different native biological membranes, and allowed molecular interaction forces, that determine protein folds and ligand binding, to be measured.

  8. Unrealistic optimism in advice taking: A computational account.

    Science.gov (United States)

    Leong, Yuan Chang; Zaki, Jamil

    2018-02-01

    Expert advisors often make surprisingly inaccurate predictions about the future, yet people heed their suggestions nonetheless. Here we provide a novel, computational account of this unrealistic optimism in advice taking. Across 3 studies, participants observed as advisors predicted the performance of a stock. Advisors varied in their accuracy, performing reliably above, at, or below chance. Despite repeated feedback, participants exhibited inflated perceptions of advisors' accuracy, and reliably "bet" on advisors' predictions more than their performance warranted. Participants' decisions tightly tracked a computational model that makes 2 assumptions: (a) people hold optimistic initial expectations about advisors, and (b) people preferentially incorporate information that adheres to their expectations when learning about advisors. Consistent with model predictions, explicitly manipulating participants' initial expectations altered their optimism bias and subsequent advice-taking. With well-calibrated initial expectations, participants no longer exhibited an optimism bias. We then explored crowdsourced ratings as a strategy to curb unrealistic optimism in advisors. Star ratings for each advisor were collected from an initial group of participants, which were then shown to a second group of participants. Instead of calibrating expectations, these ratings propagated and exaggerated the unrealistic optimism. Our results provide a computational account of the cognitive processes underlying inflated perceptions of expertise, and explore the boundary conditions under which they occur. We discuss the adaptive value of this optimism bias, and how our account can be extended to explain unrealistic optimism in other domains. (PsycINFO Database Record (c) 2018 APA, all rights reserved).

  9. Instrumental neutron activation analysis of biological samples

    International Nuclear Information System (INIS)

    Guinn, V.P.; Gavrilas, M.

    1990-01-01

    The elemental compositions of 18 biological reference materials have been processed, for 14 stepped combinations of irradiation/decay/counting times, by the INAA Advance Prediction Computer Program. The 18 materials studied include 11 plant materials, 5 animal materials, and 2 other biological materials. Of these 18 materials, 14 are NBS Standard Reference Materials and four are IAEA reference materials. Overall, the results show that a mean of 52% of the input elements can be determined to a relative standard deviation of ±10% or better by reactor flux (thermal plus epithermal) INAA

  10. Study of phosphors determination in biological samples

    International Nuclear Information System (INIS)

    Oliveira, Rosangela Magda de.

    1994-01-01

    In this paper, phosphors determination by neutron activation analysis in milk and bone samples was studied employing both instrumental and radiochemical separation methods. The analysis with radiochemistry separation consisted of the simultaneous irradiation of the samples and standards during 30 minutes, dissolution of the samples, hold back carrier, addition precipitation of phosphorus with ammonium phosphomolibdate (A.M.P.) and phosphorus-32 by counting by using Geiger-Mueller detector. The instrumental analysis consisted of the simultaneous irradiation of the samples and standards during 30 minutes, transfer of the samples into a counting planchet and measurement of the beta radiation emitted by phosphorus-32, after a suitable decay period. After the phosphorus analysis methods were established they were applied to both commercial milk and animal bone samples, and data obtained in the instrumental and radiochemical separation methods for each sample, were compared between themselves. In this work, it became possible to obtain analysis methods for phosphorus that can be applied independently of the sample quantity available, and the phosphorus content in the samples or interference that can be present in them. (author). 51 refs., 7 figs., 4 tabs

  11. Biological Sample Ambient Preservation (BioSAP) Device Project

    Data.gov (United States)

    National Aeronautics and Space Administration — To address NASA's need for alternative methods for ambient preservation of human biological samples collected during extended spaceflight and planetary operations,...

  12. Uranium-233 analysis of biological samples

    International Nuclear Information System (INIS)

    Gies, R.A.; Ballou, J.E.; Case, A.C.

    1979-01-01

    Two liquid scintillation techniques were compared for 233 U analysis: a two-phase extraction system (D2EHPA) developed by Keough and Powers, 1970, for Pu analysis; and a single-phase emulsion system (TT21) that holds the total sample in suspension with the scintillator. The first system (D2EHPA) was superior in reducing background (two- to threefold) and in accommodating a larger sample volume (fivefold). Samples containing > 50 mg/ml of slats were not extracted quantitatively by D2EHPA

  13. Commercial Fisheries Database Biological Sample (CFDBS)

    Data.gov (United States)

    National Oceanic and Atmospheric Administration, Department of Commerce — Age and length frequency data for finfish and invertebrate species collected during commercial fishing vessels. Samples are collected by fisheries reporting...

  14. Microradiagraphy of biological samples with Timepix

    Czech Academy of Sciences Publication Activity Database

    Dammer, J.; Weyda, František; Beneš, J.; Sopko, V.; Jakůbek, J.; Vondráček, V.

    2011-01-01

    Roč. 6, C11005 (2011), s. 1-6 ISSN 1748-0221. [International workshop on radiation imaging detectors /13./. Zurich, 03.07.2011-07.07.2011] R&D Projects: GA MŠk 2B06005 Grant - others:GA MŠk(CZ) LC06041; GA AV ČR(CZ) IAA600550614; GA MŠk(CZ) 2B06007; Research Program(CZ) 6840770029; Research Program(CZ) 6840770040; GA MŠk-spolupráce s CERN(CZ) 1P04LA211 Program:LC; IA; 2B; 1P Institutional research plan: CEZ:AV0Z50070508 Keywords : X- ray detectors * X- ray radiography and digital radiography (DR) * pixelated detectors and associated VLSI electronics Subject RIV: EA - Cell Biology Impact factor: 1.869, year: 2011 http://iopscience.iop.org/1748-0221/6/11/C11005/pdf/1748-0221_6_11_C11005.pdf

  15. Analytical ionic microscopic of biological samples

    International Nuclear Information System (INIS)

    Galle, P.; Rodrigues, L.E.A.

    1984-01-01

    Secondary Ion Microscopy, a microanalytical method proposed in 1960 by Castaing and Slodzian has been applied to the study of biological tissues. The main advantage of secondary ion analysis as compared to other microanalytical methods is its very high sensitivity which make it possible to detect elements even when there are at a very low concentration (0.1 ppm or less) in a microvolume, and to easily obtain images of distribution of these elements. Most stable or radioactive nuclides of every elements may be studied and the spatial resolution is of the order of 0.5μm. The present state of the art of the method and its possibility offered in biomedical research are presented. (author) [pt

  16. Contamination of biological samples by ingested sediment

    Energy Technology Data Exchange (ETDEWEB)

    Flegal, A.R.; Martin, J.H.

    1977-04-01

    An inorganic residue, presumed to be ingested sediment, was found in the rocky intertidal gastropods Tegula funebralis and Acmaea scabra and the estuarcopepods Acartia tonsa and A. clausi. When expressed as a percentage of the sample weight, this residue fraction often correlated significantly with the elemental concentrations measured in the organisms.

  17. Biological sampling for marine radioactivity monitoring

    International Nuclear Information System (INIS)

    Fowler, S.W.

    1997-01-01

    Strategies and methodologies for using marine organisms to monitor radioactivity in marine waters are presented. When the criteria for monitoring radioactivity is to determine routes of radionuclide transfer to man, the ''critical pathway'' approach is often applied. Alternatively, where information on ambient radionuclide levels and distributions is sought, the approach of selecting marine organisms as ''bioindicators'' of radioactivity is generally used. Whichever approach is applied, a great deal of knowledge is required about the physiology and ecology of the specific organism chosen. In addition, several criteria for qualifying as a bioindicator species are discussed; e.g., it must be a sedentary species which reflects the ambient radionuclide concentration at a given site, sufficiently long-lived to allow long-term temporal sampling, widely distributed to allow spatial comparisons, able to bioconcentrate the radionuclide to a relatively high degree, while showing a simple correlation between radionuclide content in its tissues with that in the surrounding waters. Useful hints on the appropriate species to use and the best way to collect and prepare organisms for radioanalysis are also given. It is concluded that benthic algae and bivalve molluscs generally offer the greatest potential for use as a ''bioindicator'' species in radionuclide biomonitoring programmes. Where knowledge on contribution to radiological dose is required, specific edible marine species should be the organisms of choice; however, both purposes can be served when the edible species chosen through critical pathway analysis is also an excellent bioaccumulator of the radionuclide of interest. (author)

  18. Micro and Nano Techniques for the Handling of Biological Samples

    DEFF Research Database (Denmark)

    Micro and Nano Techniques for the Handling of Biological Samples reviews the different techniques available to manipulate and integrate biological materials in a controlled manner, either by sliding them along a surface (2-D manipulation), or by gripping and moving them to a new position (3-D...

  19. Manipulation of biological samples using micro and nano techniques

    DEFF Research Database (Denmark)

    Castillo, Jaime; Dimaki, Maria; Svendsen, Winnie Edith

    2009-01-01

    The constant interest in handling, integrating and understanding biological systems of interest for the biomedical field, the pharmaceutical industry and the biomaterial researchers demand the use of techniques that allow the manipulation of biological samples causing minimal or no damage to thei...

  20. Neural Correlates of Realistic and Unrealistic Auditory Space Perception

    Directory of Open Access Journals (Sweden)

    Akiko Callan

    2011-10-01

    Full Text Available Binaural recordings can simulate externalized auditory space perception over headphones. However, if the orientation of the recorder's head and the orientation of the listener's head are incongruent, the simulated auditory space is not realistic. For example, if a person lying flat on a bed listens to an environmental sound that was recorded by microphones inserted in ears of a person who was in an upright position, the sound simulates an auditory space rotated 90 degrees to the real-world horizontal axis. Our question is whether brain activation patterns are different between the unrealistic auditory space (ie, the orientation of the listener's head and the orientation of the recorder's head are incongruent and the realistic auditory space (ie, the orientations are congruent. River sounds that were binaurally recorded either in a supine position or in an upright body position were served as auditory stimuli. During fMRI experiments, participants listen to the stimuli and pressed one of two buttons indicating the direction of the water flow (horizontal/vertical. Behavioral results indicated that participants could not differentiate between the congruent and the incongruent conditions. However, neuroimaging results showed that the congruent condition activated the planum temporale significantly more than the incongruent condition.

  1. Sample size and power calculation for molecular biology studies.

    Science.gov (United States)

    Jung, Sin-Ho

    2010-01-01

    Sample size calculation is a critical procedure when designing a new biological study. In this chapter, we consider molecular biology studies generating huge dimensional data. Microarray studies are typical examples, so that we state this chapter in terms of gene microarray data, but the discussed methods can be used for design and analysis of any molecular biology studies involving high-dimensional data. In this chapter, we discuss sample size calculation methods for molecular biology studies when the discovery of prognostic molecular markers is performed by accurately controlling false discovery rate (FDR) or family-wise error rate (FWER) in the final data analysis. We limit our discussion to the two-sample case.

  2. Solid-phase microextraction for the analysis of biological samples

    NARCIS (Netherlands)

    Theodoridis, G; Koster, EHM; de Jong, GJ

    2000-01-01

    Solid-phase microextraction (SPME) has been introduced for the extraction of organic compounds from environmental samples. This relatively new extraction technique has now also gained a lot of interest in a broad field of analysis including food, biological and pharmaceutical samples. SPME has a

  3. Estimation of monosaccharide radioactivity in biological samples through osazone derivatization

    Energy Technology Data Exchange (ETDEWEB)

    Garcia, F.J.; Pons, A.; Alemany, M.; Palou, A.

    1982-03-01

    A method for the quantitative estimation of radioactivity in the glucose (monosaccharide) fraction of biological samples is presented. Radioactive samples are added with cold glucose, and 1 aliquot receives a known amount of radioactive glucose as internal standard. After controlled osazone formation and three washings of the yellow precipitate, the osazones are dissolved, decolored, and their radioactivity determined through scintillation counting. The overall efficiency of recovery is 23-24% of the initial readioactivity. Each sample is corrected by the recovery of its own internal standard. There is a very close linear relationship between radioactivity present in the samples and radioactivity found, despite the use of different biological samples (rat plasma, hen egg yolk and albumen).

  4. Extraction of DNA from Forensic Biological Samples for Genotyping.

    Science.gov (United States)

    Stray, J E; Liu, J Y; Brevnov, M G; Shewale, J G

    2010-07-01

    Biological forensic samples constitute evidence with probative organic matter. Evidence believed to contain DNA is typically processed for extraction and purification of its nucleic acid content. Forensic DNA samples are composed of two things, a tissue and the substrate it resides on. Compositionally, a sample may contain almost anything and for each, the type, integrity, and content of both tissue and substrate will vary, as will the contaminant levels. This fact makes the success of extraction one of the most unpredictable steps in genotypic analysis. The development of robust genotyping systems and analysis platforms for short tandem repeat (STR) and mitochondrial DNA sequencing and the acceptance of results generated by these methods in the court system, resulted in a high demand for DNA testing. The increasing variety of sample submissions created a need to isolate DNA from forensic samples that may be compromised or contain low levels of biological material. In the past decade, several robust chemistries and isolation methods have been developed to safely and reliably recover DNA from a wide array of sample types in high yield and free of PCR inhibitors. In addition, high-throughput automated workflows have been developed to meet the demand for processing increasing numbers of samples. This review summarizes a number of the most widely adopted methods and the best practices for DNA isolation from forensic biological samples, including manual, semiautomated, and fully automated platforms. Copyright © 2010 Central Police University.

  5. Study of β-NMR for Liquid Biological Samples

    CERN Document Server

    Beattie, Caitlin

    2017-01-01

    β-NMR is an exotic form of NMR spectroscopy that allows for the characterization of matter based on the anisotropic β-decay of radioactive probe nuclei. This has been shown to be an effective spectroscopic technique for many different compounds, but its use for liquid biological samples is relatively unexplored. The work at the VITO line of ISOLDE seeks to employ this technique to study such samples. Currently, preparations are being made for an experiment to characterize DNA G-quadruplexes and their interactions with stabilizing cations. More specifically, the work in which I engaged as a summer student focused on the experiment’s liquid handling system and the stability of the relevant biological samples under vacuum.

  6. Efficient sample preparation from complex biological samples using a sliding lid for immobilized droplet extractions.

    Science.gov (United States)

    Casavant, Benjamin P; Guckenberger, David J; Beebe, David J; Berry, Scott M

    2014-07-01

    Sample preparation is a major bottleneck in many biological processes. Paramagnetic particles (PMPs) are a ubiquitous method for isolating analytes of interest from biological samples and are used for their ability to thoroughly sample a solution and be easily collected with a magnet. There are three main methods by which PMPs are used for sample preparation: (1) removal of fluid from the analyte-bound PMPs, (2) removal of analyte-bound PMPs from the solution, and (3) removal of the substrate (with immobilized analyte-bound PMPs). In this paper, we explore the third and least studied method for PMP-based sample preparation using a platform termed Sliding Lid for Immobilized Droplet Extractions (SLIDE). SLIDE leverages principles of surface tension and patterned hydrophobicity to create a simple-to-operate platform for sample isolation (cells, DNA, RNA, protein) and preparation (cell staining) without the need for time-intensive wash steps, use of immiscible fluids, or precise pinning geometries. Compared to other standard isolation protocols using PMPs, SLIDE is able to perform rapid sample preparation with low (0.6%) carryover of contaminants from the original sample. The natural recirculation occurring within the pinned droplets of SLIDE make possible the performance of multistep cell staining protocols within the SLIDE by simply resting the lid over the various sample droplets. SLIDE demonstrates a simple easy to use platform for sample preparation on a range of complex biological samples.

  7. BSPS Program (ESI-Mass Spectrometry) Biological Sample Data Analysis; Disruption of Bacteria Spores

    National Research Council Canada - National Science Library

    Lall, Ravi P

    2005-01-01

    The various biological processing technologies and biological identification approaches are essential for support of the mission to develop and demonstrate an advanced Biological Sample Preparation System...

  8. Sampling and sample preparation methods for the analysis of trace elements in biological material

    International Nuclear Information System (INIS)

    Sansoni, B.; Iyengar, V.

    1978-05-01

    The authors attempt to give a most systamtic possible treatment of the sample taking and sample preparation of biological material (particularly in human medicine) for trace analysis (e.g. neutron activation analysis, atomic absorption spectrometry). Contamination and loss problems are discussed as well as the manifold problems of the different consistency of solid and liquid biological materials, as well as the stabilization of the sample material. The process of dry and wet ashing is particularly dealt with, where new methods are also described. (RB) [de

  9. Apparatus for freeze drying of biologic and sediment samples

    International Nuclear Information System (INIS)

    Anon.

    1978-01-01

    Freeze drying to obtain water from individual samples, though not complicated, usually requires considerable effort to maintain the cold traps on a 24-hr basis. In addition, the transfer of a sample from sample containers to freeze-dry flasks is usually made with some risk of contamination to the sample. If samples are large, 300 g to 600 g, usually several days are required to dry the samples. The use of an unattended system greatly improves personnel and drying efficiency. Commercial freeze dryers are not readily applicable to the problems of collecting water from individual samples, and lab-designed collectors required sample transfer and continual replenishment of the dry ice. A freeze-dry apparatus for collecting water from individual sediment and/or biological samples was constructed to determine the tritium concentrations in fish for dose calcaluations and the tritium distribution in sediment cores for water movement studies. The freeze, dry apparatus, which can handle eight samples simultaneously and conveniently, is set up for unattended 24-hr operation and is designed to avoid sample transfer problems

  10. A large-scale cryoelectronic system for biological sample banking

    Science.gov (United States)

    Shirley, Stephen G.; Durst, Christopher H. P.; Fuchs, Christian C.; Zimmermann, Heiko; Ihmig, Frank R.

    2009-11-01

    We describe a polymorphic electronic infrastructure for managing biological samples stored over liquid nitrogen. As part of this system we have developed new cryocontainers and carrier plates attached to Flash memory chips to have a redundant and portable set of data at each sample. Our experimental investigations show that basic Flash operation and endurance is adequate for the application down to liquid nitrogen temperatures. This identification technology can provide the best sample identification, documentation and tracking that brings added value to each sample. The first application of the system is in a worldwide collaborative research towards the production of an AIDS vaccine. The functionality and versatility of the system can lead to an essential optimization of sample and data exchange for global clinical studies.

  11. Perceptions of control and unrealistic optimism in early-phase cancer trials.

    Science.gov (United States)

    Jansen, Lynn A; Mahadevan, Daruka; Appelbaum, Paul S; Klein, William M P; Weinstein, Neil D; Mori, Motomi; Degnin, Catherine; Sulmasy, Daniel P

    2018-02-01

    Recent research has found unrealistic optimism (UO) among patient-subjects in early-phase oncology trials. Our aim was to investigate the cognitive and motivational factors that evoke this bias in this context. We expected perceptions of control to be a strong correlate of unrealistic optimism. A study of patient-subjects enrolled in early-phase oncology trials was conducted at two sites in the USA. Respondents completed questionnaires designed to assess unrealistic optimism and several risk attribute variables that have been found to evoke the bias in other contexts. One hundred and seventy-one patient-subjects agreed to be interviewed for our study. Significant levels of perceived controllability were found with respect to all nine research-related questions. Perceptions of control were found to predict unrealistic optimism. Two other risk attribute variables, awareness of indicators (p=0.024) and mental image (p=0.022), were correlated with unrealistic optimism. However, in multivariate regression analysis, awareness and mental image dropped out of the model and perceived controllability was the only factor independently associated with unrealistic optimism (poptimism about benefiting personally from trial participation. Effective interventions to counteract unrealistic optimism may need to address the psychological factors that give rise to distorted risk/benefit processing. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2018. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

  12. Toxicological Analysis of Some Drugs of Abuse in Biological Samples

    Directory of Open Access Journals (Sweden)

    Anne Marie Ciobanu

    2015-10-01

    Full Text Available Consumption of drugs of abuse is a scourge of modern world. Abuse, drug addiction and their consequences are one of the major current problems of European society because of the significant repercussions in individual, family, social and economic level. In this context, toxicological analysis of the drugs of abuse in biological samples is a useful tool for: diagnosis of drug addiction, checking an auto-response, mandatory screening in some treatment programs, identification of a substance in the case of an overdose, determining compliance of the treatment. The present paper aims to address the needs of healthcare professionals involved in drugs addiction treatment through systematic presentation of information regarding their toxicological analysis. Basically, it is a tool that help you to select the suitable biological sample and the right collecting time, as well as the proper analysis technique, depending on the purpose of analysis, pharmacokinetic characteristics of the drugs of abuse, available equipment and staff expertise.

  13. CeDAMar global database of abyssal biological sampling

    OpenAIRE

    Stuart, Carol T.; Arbizu, Pedro Martinez; Smith, Craig R.; Molodtsova, Tina; Brandt, Angelika; Etter, Ron J.; Escobar-briones, Elva; Fabri, Marie-claire; Rex, Michael A.

    2008-01-01

    The Census of the Diversity of Abyssal Marine Life (CeDAMar), a division of the Census of Marine Life, has compiled the first comprehensive global database of biological samples taken in the abyssal plains of the world ocean. It is an essential resource for planning future exploration of the abyss, for synthesizing patterns of biogeography and biodiversity, and for environmentally safe exploitation of natural resources. The database is described in this article, and made available to investig...

  14. [Progress on Determination and Analysis of Zopiclone in Biological Samples].

    Science.gov (United States)

    Shu, C X; Gong, D; Zhang, L P; Zhao, J X

    2017-12-01

    As a new hypnotic, zopiclone is widely used in clinical treatment. There are many methods for determination of zopiclone, including spectrophotometry, chromatography and chromatography mass spectrum, etc. Present paper reviews different kinds of biological samples associated with zopiclone, extraction and purification methods, and determination and analysis methods, which aims to provide references for the relevant research and practice. Copyright© by the Editorial Department of Journal of Forensic Medicine.

  15. Analytical methodologies for the determination of benzodiazepines in biological samples.

    Science.gov (United States)

    Persona, Karolina; Madej, Katarzyna; Knihnicki, Paweł; Piekoszewski, Wojciech

    2015-09-10

    Benzodiazepine drugs belong to important and most widely used medicaments. They demonstrate such therapeutic properties as anxiolytic, sedative, somnifacient, anticonvulsant, diastolic and muscle relaxant effects. However, despite the fact that benzodiazepines possess high therapeutic index and are considered to be relatively safe, their use can be dangerous when: (1) co-administered with alcohol, (2) co-administered with other medicaments like sedatives, antidepressants, neuroleptics or morphine like substances, (3) driving under their influence, (4) using benzodiazepines non-therapeutically as drugs of abuse or in drug-facilitated crimes. For these reasons benzodiazepines are still studied and determined in a variety of biological materials. In this article, sample preparation techniques which have been applied in analysis of benzodiazepine drugs in biological samples have been reviewed and presented. The next part of the article is focused on a review of analytical methods which have been employed for pharmacological, toxicological or forensic study of this group of drugs in the biological matrices. The review was preceded by a description of the physicochemical properties of the selected benzodiazepines and two, very often coexisting in the same analyzed samples, sedative-hypnotic drugs. Copyright © 2015. Published by Elsevier B.V.

  16. Determination of platinum in biological samples by NAA

    International Nuclear Information System (INIS)

    Okada, Yukiko; Hirai, Shoji; Sakurai, Hiromu; Haraguchi, Hiroki.

    1990-01-01

    Recently, a Pt compound, Cisplatin (cis-dichlorodiamine platinum) has been used therapeutically as an effective anti-malignant-cancer drug. However, since this drug has a harmful aftereffect on kidney, an urgent study of how to reduce its toxicity without influencing the therapeutic effect is needed. We have to understand the behavior of Pt in biological organs in order to elucidate the mechanism of its toxicity reduction. In this study, the analytical conditions for the determination of Pt in biological samples by neutron activation analysis, such as cooling time, counting time and sample weight, are optimized. Freeze-dried samples of the liver, kidney and whole blood of a rat treated with Cisplatin were prepared to evaluate the precision of the analysis and the lower limit of determination. 199 Au (t 1/2 = 3.15 d) produced from 199 Pt (n, γ, β - ) was selected as the analytical radionuclide. A concentration of ca. 1 ppm Pt was determinable under the optimal conditions: a cooling time of 5 d and a counting time of 1 h. Pt in the respective organs of the control rat was not detected under the same analytical conditions. The concentrations of Pt in the liver, kidney, spleen, pancreas and lung of a rat treated with both Cisplatin and sodium selenite were higher than those of a rat treated only with Cisplatin. (author)

  17. Using biological samples in epidemiological research on drugs of abuse

    Directory of Open Access Journals (Sweden)

    Hallvard Gjerde

    2011-12-01

    Full Text Available Blood, oral fluid (saliva, urine and hair are the most commonly used biological matrices for drug testing in epidemiological drug research. Other biological matrices may also be used for selected purposes. Blood reflects recent drug intake and may be used to assess impairment. Oral fluid reflects drug presence in blood and thereby also recent intake, but drug concentrations in this matrix cannot be used to accurately estimate concentrations in blood. Urine reflects drug use during the last few days and in some cases for a longer period, but does not indicate the dose size or frequency of use. Hair reflects drug use during several months, but is a poor matrix for detecting use of cannabis. If using a single drug dose, this can be detected in blood and urine if the sample is taken within the detection timeframes, in most cases also in oral fluid. Single drug use is most often insufficient for producing a positive test result in a sample of hair. For cocaine and amphetamine, weekly use may be needed, while for cannabis a positive result is not guaranteed even after daily use. Refusal rates are lowest for oral fluid and highest for blood and hair samples. The analytical costs are lowest for urine and highest for hair. Combined use of questionnaires/interviews and drug testing detects more drug use than when using only one of those methods and is therefore expected to give more accurate data.

  18. Spectrophotometric determination of vanadium in environmental and biological samples

    International Nuclear Information System (INIS)

    Rekha, D.; Krishnapriya, B.; Subrahmanyam, P.; Reddyprasad, P.; Dilip Kumar, J.; Chiranjeevi, P.

    2007-01-01

    The method is based on oxidation of p-nitro aniline by vanadium (V) followed by coupling reaction with N-(1-naphthalene-1-y1)ethane-1, 2-diaminedihydrochloride (NEDA) in basic medium of pH 8 to give purple colored derivative. The derivative having an λ max 525nm is stable for 10 days. Beer's law is obeyed for vanadium (V) in the concentration range of 0.03-4.5 μg ml -1 . The proposed method was successfully applied to the analysis of vanadium in environmental and biological samples. (author)

  19. Analysis of biological samples for americium and curium

    International Nuclear Information System (INIS)

    Miglio, J.J.

    1976-01-01

    A method of analyzing biological materials by liquid scintillation counting for americium and curium which greatly reduces the contribution from 40 K is described. The method employs an extractant liquid scintillation cocktail using N,N,N-trioctyl-N-methyl-ammonium chloride as the extractant. Instrument as well as tissue backgrounds are reduced. The lowered backgrounds allow picocurie level samples to be analyzed by liquid scintillation counting instead of alpha pulse height analysis. The samples are reduced to a carbon-free ash and then dissolved in 8M LiNo 3 which is also 10 -2 M in HNO 3 . An aliquot is placed in a liquid scintillation vial along with the extractant-scintillator, shaken and counted

  20. A low temperature scanning force microscope for biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Gustafsson, Mats Gustaf Lennart [Univ. of California, Berkeley, CA (United States)

    1993-05-01

    An SFM has been constructed capable of operating at 143 K. Two contributions to SFM technology are described: a new method of fabricating tips, and new designs of SFM springs that significantly lower the noise level. The SFM has been used to image several biological samples (including collagen, ferritin, RNA, purple membrane) at 143 K and room temperature. No improvement in resolution resulted from 143 K operation; several possible reasons for this are discussed. Possibly sharper tips may help. The 143 K SFM will allow the study of new categories of samples, such as those prepared by freeze-frame, single molecules (temperature dependence of mechanical properties), etc. The SFM was used to cut single collagen molecules into segments with a precision of {le} 10 nm.

  1. Microsystem strategies for sample preparation in biological detection.

    Energy Technology Data Exchange (ETDEWEB)

    James, Conrad D.; Galambos, Paul C.; Bennett, Dawn Jonita (University of Maryland Baltimore County, Baltimore, MD); Manginell, Monica; Okandan, Murat; Acrivos, Andreas (The City College of New York, NY); Brozik, Susan Marie; Khusid, Boris (New Jersey Institute of Technology, Newark, NJ)

    2005-03-01

    The objective of this LDRD was to develop microdevice strategies for dealing with samples to be examined in biological detection systems. This includes three sub-components: namely, microdevice fabrication, sample delivery to the microdevice, and sample processing within the microdevice. The first component of this work focused on utilizing Sandia's surface micromachining technology to fabricate small volume (nanoliter) fluidic systems for processing small quantities of biological samples. The next component was to develop interfaces for the surface-micromachined silicon devices. We partnered with Micronics, a commercial company, to produce fluidic manifolds for sample delivery to our silicon devices. Pressure testing was completed to examine the strength of the bond between the pressure-sensitive adhesive layer and the silicon chip. We are also pursuing several other methods, both in house and external, to develop polymer-based fluidic manifolds for packaging silicon-based microfluidic devices. The second component, sample processing, is divided into two sub-tasks: cell collection and cell lysis. Cell collection was achieved using dielectrophoresis, which employs AC fields to collect cells at energized microelectrodes, while rejecting non-cellular particles. Both live and dead Staph. aureus bacteria have been collected using RF frequency dielectrophoresis. Bacteria have been separated from polystyrene microspheres using frequency-shifting dielectrophoresis. Computational modeling was performed to optimize device separation performance, and to predict particle response to the dielectrophoretic traps. Cell lysis is continuing to be pursued using microactuators to mechanically disrupt cell membranes. Novel thermal actuators, which can generate larger forces than previously tested electrostatic actuators, have been incorporated with and tested with cell lysis devices. Significant cell membrane distortion has been observed, but more experiments need to be

  2. Atypical antipsychotics: trends in analysis and sample preparation of various biological samples.

    Science.gov (United States)

    Fragou, Domniki; Dotsika, Spyridoula; Sarafidou, Parthena; Samanidou, Victoria; Njau, Samuel; Kovatsi, Leda

    2012-05-01

    Atypical antipsychotics are increasingly popular and increasingly prescribed. In some countries, they can even be obtained over-the-counter, without a prescription, making their abuse quite easy. Although atypical antipsychotics are thought to be safer than typical antipsychotics, they still have severe side effects. Intoxications are not rare and some of them have a fatal outcome. Drug interactions involving atypical antipsychotics complicate patient management in clinical settings and the determination of the cause of death in fatalities. In view of the above, analytical strategies that can efficiently isolate atypical antipsychotics from a variety of biological samples and quantify them accurately, sensitively and reliably, are of utmost importance both for the clinical, as well as for the forensic toxicologist. In this review, we will present and discuss novel analytical strategies that have been developed from 2004 to the present day for the determination of atypical antipsychotics in various biological samples.

  3. Proteomic challenges: sample preparation techniques for microgram-quantity protein analysis from biological samples.

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B

    2015-02-05

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed.

  4. Proteomic Challenges: Sample Preparation Techniques for Microgram-Quantity Protein Analysis from Biological Samples

    Science.gov (United States)

    Feist, Peter; Hummon, Amanda B.

    2015-01-01

    Proteins regulate many cellular functions and analyzing the presence and abundance of proteins in biological samples are central focuses in proteomics. The discovery and validation of biomarkers, pathways, and drug targets for various diseases can be accomplished using mass spectrometry-based proteomics. However, with mass-limited samples like tumor biopsies, it can be challenging to obtain sufficient amounts of proteins to generate high-quality mass spectrometric data. Techniques developed for macroscale quantities recover sufficient amounts of protein from milligram quantities of starting material, but sample losses become crippling with these techniques when only microgram amounts of material are available. To combat this challenge, proteomicists have developed micro-scale techniques that are compatible with decreased sample size (100 μg or lower) and still enable excellent proteome coverage. Extraction, contaminant removal, protein quantitation, and sample handling techniques for the microgram protein range are reviewed here, with an emphasis on liquid chromatography and bottom-up mass spectrometry-compatible techniques. Also, a range of biological specimens, including mammalian tissues and model cell culture systems, are discussed. PMID:25664860

  5. Determination of total mercury in biological and geological samples

    Science.gov (United States)

    Crock, James G.

    2005-01-01

    The analytical chemist is faced with several challenges when determining mercury in biological and geological materials. These challenges include widespread mercury contamination, both in the laboratory and the environment, possible losses of mercury during sample preparation and digestion, the wide range of mercury values commonly observed, ranging from the low nanogram per gram or per liter for background areas to hundreds of milligrams per kilogram in contaminated or ore-bearing areas, great matrix diversity, and sample heterogeneity1. These factors can be naturally occurring or anthropogenic, but must be addressed to provide a precise and accurate analysis. Although there are many instrumental methods available for the successful determination of mercury, no one technique will address all problems or all samples all of the time. The approach for the determination of mercury used at the U.S. Geological Survey, Crustal Imaging and Characterization Team, Denver Laboratories, utilizes a suite of complementary instrumental methods when approaching a study requiring mercury analyses. Typically, a study could require the analysis of waters, leachates or selective digestions of solids, vegetation, and biological materials such as tissue, bone, or shell, soils, rocks, sediments, coals, sludges, and(or) ashes. No one digestion or sample preparation method will be suitable for all of these matrices. The digestions typically employed at our laboratories include: (i) a closed-vessel microwave method using nitric acid and hydrogen peroxide, followed by digestion/dilution with a nitric acid/sodium dichromate solution, (ii) a robotic open test-tube digestion with nitric acid and sodium dichromate, (iii) a sealed Teflon? vessel with nitric acid and sodium dichromate, (iv) a sealed glass bottle with nitric acid and sodium dichromate, or (v) open test tube digestion with nitric and sulfuric acids and vanadium pentoxide. The common factor in all these digestions is that they are

  6. Analysis of boron containing biological samples by ICP

    International Nuclear Information System (INIS)

    Bauer, W.F.; Johnson, D.A.; Messick, K.M.; Miller, D.L.; Propp, W.A.; Steele, S.M.

    1988-01-01

    An important aspect of boron neutron capture therapy (BNCT) is the determination of the biological distribution of the boron within an organism at some point in time after administration of a boron- containing species. Techniques include prompt gamma analysis, colorimetric techniques, and most recently, inductively coupled plasma atomic emission spectroscopy (ICP-AES) techniques. In this paper, an ICP technique was used to determine the boron content in tissue and various biological fluid samples obtained from dogs have spontaneously-occurring brain tumors and to which had been administered the sodium salt of the sulfhydryl borane (B 12 H 11 SH)/sup 2/minus//. The spontaneous error model allowed tissue to be collected that had the same relative kinetics and disruptions of the blood brain barrier as found in human brain cancer. Many of these subjects also had peritumor edematous tissue that did not have a visibly detected alteration in the blood brain barrier. The large size of the dog allowed tissues to be collected for analysis that may be affected during irradiation

  7. Micro-radiography of biological samples with medical contrast agents

    Science.gov (United States)

    Dammer, J.; Weyda, F.; Benes, J.; Sopko, V.; Gelbic, I.

    2013-12-01

    Micro-radiography is an imaging technique that uses X-rays to study the internal structures of objects. This fast and easy imaging tool is based on differential X-ray attenuation by various tissues and structures within biological samples. The experimental setup described is based on the semiconductor pixel X-ray detector Medipix2 and X-ray micro-focus tube. Our micro-radiographic system has been recently used not only for the examination of internal structures of various arthropods and other biological objects but also for tracing some processes in selected model species (we used living larvae of mosquito Culex quinquefasciatus). Low concentrations of iodine, lanthanum or gold particles were used as a tracer (contrast agent). Such contrast agents increase the absorption of X-rays and allow a better visibility of internal structures of model organisms (especially the various cavities, pores, etc.). In addition, the movement of tracers in selected timing experiments demonstrates some physiological functions of digestive and excretory system.

  8. Variations in Unrealistic Optimism Between Acceptors and Decliners of Early Phase Cancer Trials.

    Science.gov (United States)

    Jansen, Lynn A; Mahadevan, Daruka; Appelbaum, Paul S; Klein, William M P; Weinstein, Neil D; Mori, Motomi; Degnin, Catherine; Sulmasy, Daniel P

    2017-10-01

    Research has found that patient-subjects in early phase cancer trials exhibit unrealistic optimism regarding the risks and possible benefits of trial participation. Unrealistic optimism is associated with therapeutic misconception and failures to appreciate research-related information. This is the first study to assess whether those who decline to participate in these trials also exhibit unrealistic optimism. It is also the first study to assess whether there are significant differences in appreciation of research-related risks/benefits and therapeutic misconception between these two groups. We approached 261 patients at two academic medical centers who were offered enrollment in a Phase I, II, or I/II cancer trial (between 2012 and 2016). Two hundred thirty-three patients agreed to enroll in an early phase cancer trial, 171 of whom agreed to be interviewed for the study. Twenty-eight patients declined the offer to enroll, 15 of whom agreed to be interviewed for the study. Subjects participated in a structured face-to-face interview with a research associate trained to administer the study questionnaires. Acceptors demonstrated a significantly higher level of unrealistic optimism than decliners ( p optimism is consequential for the decision to participate in these trials. The different levels of unrealistic optimism exhibited by these groups suggest that it may be a factor that affects the decision to participate.

  9. Digital holography microscopy in 3D biologic samples analysis

    Energy Technology Data Exchange (ETDEWEB)

    Ricardo, J O; Palacios, F; Palacios, G F; Sanchez, A [Department of Physics, University of Oriente (Cuba); Muramatsu, M [Department of General Physics, University of Sao Paulo - Sao Paulo (Brazil); Gesualdi, M [Engineering center, Models and Applied Social Science, UFABC - Sao Paulo (Brazil); Font, O [Department of Bio-ingeniering, University of Oriente - Santiago de Cuba (Cuba); Valin, J L [Mechanics Department, ISPJAE, Habana (Cuba); Escobedo, M; Herold, S [Department of Computation, University of Oriente (Cuba); Palacios, D F, E-mail: frpalaciosf@gmail.com [Department of Nuclear physics, University of Simon BolIva (Venezuela, Bolivarian Republic of)

    2011-01-01

    In this work it is used a setup for Digital Holography Microscopy (MHD) for 3D biologic samples reconstruction. The phase contrast image reconstruction is done by using the Double propagation Method. The system was calibrated and tested by using a micrometric scale and pure phase object respectively. It was simulated the human red blood cell (erythrocyte) and beginning from the simulated hologram the digital 3D phase image for erythrocytes it was calculated. Also there was obtained experimental holograms of human erythrocytes and its corresponding 3D phase images, being evident the correspondence qualitative and quantitative between these characteristics in the simulated erythrocyte and in the experimentally calculated by DHM in both cases.

  10. [Psychoactive substances in biological samples--toxicological laboratory data].

    Science.gov (United States)

    Gomółka, Ewa; Wilimowska, Jolanta; Piekoszewski, Wojciech; Groszek, Barbara

    2004-01-01

    The subject of the research was the analysis of frequency and type of psychoactive substances used, basing on the determinations the blood and/or urine samples, performed in the toxicological laboratory of the Department of Clinical and Industrial Toxicology Jagiellonian University in Kraków in the period from December 2001 to November 2003. From 17,649 performed determinations--45.5% were positive. 50% of the positive determinations were psychoactive substances. The most often psychoactive substance determined was ethyl alcohol (52.86%), next benzodiazepines (17.41%), amphetamines (10.54%), opiates (8.05%), THC (6.87%), barbiturates (3.74%), and occasionally atropine and cocaine. There was observed a variety of mixed, simultaneously taking psychoactive substances, especially ethyl alcohol, opiates, amphetamine derivatives and cannabinoids. The analysis of the occurrence of psychoactive substances in biological samples from patients treated in different hospital departments, others hospitals and ordered by private persons also was performed. In the last two years 369 private patients ordered psychoactive substances determinations and 78 of them were positive.

  11. Scanning Ion Conductance Microscopy for Studying Biological Samples

    Directory of Open Access Journals (Sweden)

    Irmgard D. Dietzel

    2012-11-01

    Full Text Available Scanning ion conductance microscopy (SICM is a scanning probe technique that utilizes the increase in access resistance that occurs if an electrolyte filled glass micro-pipette is approached towards a poorly conducting surface. Since an increase in resistance can be monitored before the physical contact between scanning probe tip and sample, this technique is particularly useful to investigate the topography of delicate samples such as living cells. SICM has shown its potential in various applications such as high resolution and long-time imaging of living cells or the determination of local changes in cellular volume. Furthermore, SICM has been combined with various techniques such as fluorescence microscopy or patch clamping to reveal localized information about proteins or protein functions. This review details the various advantages and pitfalls of SICM and provides an overview of the recent developments and applications of SICM in biological imaging. Furthermore, we show that in principle, a combination of SICM and ion selective micro-electrodes enables one to monitor the local ion activity surrounding a living cell.

  12. Automated force volume image processing for biological samples.

    Directory of Open Access Journals (Sweden)

    Pavel Polyakov

    2011-04-01

    Full Text Available Atomic force microscopy (AFM has now become a powerful technique for investigating on a molecular level, surface forces, nanomechanical properties of deformable particles, biomolecular interactions, kinetics, and dynamic processes. This paper specifically focuses on the analysis of AFM force curves collected on biological systems, in particular, bacteria. The goal is to provide fully automated tools to achieve theoretical interpretation of force curves on the basis of adequate, available physical models. In this respect, we propose two algorithms, one for the processing of approach force curves and another for the quantitative analysis of retraction force curves. In the former, electrostatic interactions prior to contact between AFM probe and bacterium are accounted for and mechanical interactions operating after contact are described in terms of Hertz-Hooke formalism. Retraction force curves are analyzed on the basis of the Freely Jointed Chain model. For both algorithms, the quantitative reconstruction of force curves is based on the robust detection of critical points (jumps, changes of slope or changes of curvature which mark the transitions between the various relevant interactions taking place between the AFM tip and the studied sample during approach and retraction. Once the key regions of separation distance and indentation are detected, the physical parameters describing the relevant interactions operating in these regions are extracted making use of regression procedure for fitting experiments to theory. The flexibility, accuracy and strength of the algorithms are illustrated with the processing of two force-volume images, which collect a large set of approach and retraction curves measured on a single biological surface. For each force-volume image, several maps are generated, representing the spatial distribution of the searched physical parameters as estimated for each pixel of the force-volume image.

  13. "If a Lion Could Speak ...": Online Sensitivity to Propositional Truth-Value of Unrealistic Counterfactual Sentences

    Science.gov (United States)

    Nieuwland, Mante S.

    2013-01-01

    People can establish whether a sentence is hypothetically true even if what it describes can never be literally true given the laws of the natural world. Two event-related potential (ERP) experiments examined electrophysiological responses to sentences about unrealistic counterfactual worlds that require people to construct novel conceptual…

  14. Concurrently examining unrealistic absolute and comparative optimism: Temporal shifts, individual-difference and event-specific correlates, and behavioural outcomes.

    Science.gov (United States)

    Ruthig, Joelle C; Gamblin, Bradlee W; Jones, Kelly; Vanderzanden, Karen; Kehn, Andre

    2017-02-01

    Researchers have spent considerable effort examining unrealistic absolute optimism and unrealistic comparative optimism, yet there is a lack of research exploring them concurrently. This longitudinal study repeatedly assessed unrealistic absolute and comparative optimism within a performance context over several months to identify the degree to which they shift as a function of proximity to performance and performance feedback, their associations with global individual difference and event-specific factors, and their link to subsequent behavioural outcomes. Results showed similar shifts in unrealistic absolute and comparative optimism based on proximity to performance and performance feedback. Moreover, increases in both types of unrealistic optimism were associated with better subsequent performance beyond the effect of prior performance. However, several differences were found between the two forms of unrealistic optimism in their associations with global individual difference factors and event-specific factors, highlighting the distinctiveness of the two constructs. © 2016 The British Psychological Society.

  15. Inter comparison of 90Sr and 137Cs contents in biologic samples and natural U in soil samples

    International Nuclear Information System (INIS)

    Liu Jianfen; Zeng Guangjian; Lu Xuequan

    2001-01-01

    The results of the 90 Sr and 137 Cs contents in biologic samples and the natural U in soil samples obtained in a joint effort by fourteen environmental radiation laboratories in the Chinese environmental protection system were analyzed and compared. Two kinds of biologic samples and one kind of soil samples were used for inter comparison. Of which, one kind of biologic samples (biologic powder samples) and the soil samples came from the IAEA samples were environmental and the reference values were known. The another kind of biologic samples were environmental tea-leaf that were taken from a tea garden near Hangzhou. The mean values obtained by all the joined laboratories was used as the reference. The inter comparison results were expressed in terms of the deviation from the reference value. It was found that the deviation of the 90 Sr and 137 Cs contents of biologic powder samples ranged from -15.4% to 26.5% and -15.0% to 0.4%, respectively. The deviation of the natural U content ranged from -25.5% to 7.3% for the soil samples. For the tea-leaf, the 90 Sr deviation was -22.7% to 19.1%, and the 137 Cs data had a relative large scatter with a ratio of the maximum and the minimum values being about 7. It was pointed out that the analysis results offered by different laboratories might have involved system errors

  16. Amchitka Island, Alaska, Biological Monitoring Report 2011 Sampling Results

    Energy Technology Data Exchange (ETDEWEB)

    None

    2013-09-01

    The Long-Term Surveillance and Maintenance (LTS&M) Plan for the U.S. Department of Energy (DOE) Office of Legacy Management (LM) Amchitka Island sites describes how LM plans to conduct its mission to protect human health and the environment at the three nuclear test sites located on Amchitka Island, Alaska. Amchitka Island, near the western end of the Aleutian Islands, is approximately 1,340 miles west-southwest of Anchorage, Alaska. Amchitka is part of the Aleutian Island Unit of the Alaska Maritime National Wildlife Refuge, which is administered by the U.S. Fish and Wildlife Service (USFWS). Since World War II, Amchitka has been used by multiple U.S. government agencies for various military and research activities. From 1943 to 1950, it was used as a forward air base for the U.S. Armed Forces. During the middle 1960s and early 1970s, the U.S. Department of Defense (DOD) and the U.S. Atomic Energy Commission (AEC) used a portion of the island as a site for underground nuclear tests. During the late 1980s and early 1990s, the U.S. Navy constructed and operated a radar station on the island. Three underground nuclear tests were conducted on Amchitka Island. DOD, in conjunction with AEC, conducted the first nuclear test (named Long Shot) in 1965 to provide data that would improve the United States' capability of detecting underground nuclear explosions. The second nuclear test (Milrow) was a weapons-related test conducted by AEC in 1969 as a means to study the feasibility of detonating a much larger device. Cannikin, the third nuclear test on Amchitka, was a weapons-related test detonated on November 6, 1971. With the exception of small concentrations of tritium detected in surface water shortly after the Long Shot test, radioactive fission products from the tests remain in the subsurface at each test location As a continuation of the environmental monitoring that has taken place on Amchitka Island since before 1965, LM in the summer of 2011 collected biological

  17. Tempting fate or inviting happiness?: unrealistic idealization prevents the decline of marital satisfaction.

    Science.gov (United States)

    Murray, Sandra L; Griffin, Dale W; Derrick, Jaye L; Harris, Brianna; Aloni, Maya; Leder, Sadie

    2011-05-01

    This article examines whether unrealistically viewing a romantic partner as resembling one's ideal partner accelerates or slows declines in marital satisfaction among newlyweds. A longitudinal study linked unrealistic idealization at the time of marriage to changes in satisfaction over the first 3 years of marriage. Overall, satisfaction declined markedly, a finding that is consistent with past research. However, seeing a less-than-ideal partner as a reflection of one's ideals predicted a certain level of protection against the corrosive effects of time: People who initially idealized their partner the most experienced no decline in satisfaction. The benefits of idealization remained in analyses that controlled separately for the positivity of partner perceptions and the possibility that better adjusted people might be in better relationships.

  18. Tempting Fate or Inviting Happiness? Unrealistic idealization prevents the decline of marital satisfaction

    Science.gov (United States)

    Murray, Sandra L.; Griffin, Dale W.; Derrick, Jaye L.; Harris, Brianna; Aloni, Maya; Leder, Sadie

    2014-01-01

    The authors examine whether unrealistically viewing a romantic partner as the image of one’s ideal partner accelerates or slows declines in marital satisfaction among newlyweds. A longitudinal study linked unrealistic idealization at the point of marriage to changes in satisfaction over the first three years of marriage. Overall, satisfaction declined markedly, consistent with past research. However, seeing a less-than-ideal partner as a reflection of one’s ideals predicted a certain level of immunity to the corrosive effects of time: People who initially idealized their partner highly experienced no declines in satisfaction. The obtained benefits of idealization remained in analyses that separately controlled for the positivity of partner perceptions and the possibility that better adjusted people might be in better relationships. PMID:21467549

  19. Unrealistic comparative optimism: An unsuccessful search for evidence of a genuinely motivational bias.

    Science.gov (United States)

    Harris, Adam J L; de Molière, Laura; Soh, Melinda; Hahn, Ulrike

    2017-01-01

    One of the most accepted findings across psychology is that people are unrealistically optimistic in their judgments of comparative risk concerning future life events-they judge negative events as less likely to happen to themselves than to the average person. Harris and Hahn (2011), however, demonstrated how unbiased (non-optimistic) responses can result in data patterns commonly interpreted as indicative of optimism due to statistical artifacts. In the current paper, we report the results of 5 studies that control for these statistical confounds and observe no evidence for residual unrealistic optimism, even observing a 'severity effect' whereby severe outcomes were overestimated relative to neutral ones (Studies 3 & 4). We conclude that there is no evidence supporting an optimism interpretation of previous results using the prevalent comparison method.

  20. SOCIAL-COMPARISON OF HEALTH RISKS - LOCUS OF CONTROL, THE PERSON-POSITIVITY BIAS, AND UNREALISTIC OPTIMISM

    NARCIS (Netherlands)

    HOORENS, [No Value; BUUNK, BP

    1993-01-01

    People typically attribute lower health risks to themselves than to others, a phenomenon referred to as unrealistic optimism. The present study tested the person positivity bias as a previously unexamined explanation of the phenomenon and analyzed the relationship between unrealistic optimism and

  1. Microradiography of biological samples with medici kontrast agents

    Czech Academy of Sciences Publication Activity Database

    Dammer, J.; Weyda, F.; Beneš, J.; Sopko, V.; Gelbič, Ivan

    2013-01-01

    Roč. 730, DEC 1 (2013), s. 149-151 ISSN 0168-9002 Institutional support: RVO:60077344 Keywords : X-ray detectors * X-ray radiography and digital radiography * inspection with X-rays Subject RIV: EA - Cell Biology Impact factor: 1.316, year: 2013

  2. The measurement of radioactive microspheres in biological samples

    International Nuclear Information System (INIS)

    Mernagh, J.R.; Spiers, E.W.; Adiseshiah, M.

    1976-01-01

    Measurements of the distribution of radioactive microspheres are used in investigations of regional coronary blood flow, but the size and shape of the heart varies for different test animals, and the organ is frequently divided into smaller pieces for studies of regional perfusion. Errors are introduced by variations in the distribution of the radioactive source and the amount of Compton scatter in different samples. A technique has therefore been developed to allow the counting of these tissue samples in their original form, and correction factors have been derived to inter-relate the various counting geometries thus encountered. Dogs were injected with microspheres labelled with 141 Ce, 51 Cr or 85 Sr. The tissue samples did not require remodelling to fit a standard container, and allowance was made for the inhomogeneous distribution in the blood samples. The activities in the centrifuged blood samples were correlated with those from the tissue samples by a calibration procedure involving comparisons of the counts from samples of microspheres embedded in sachets of gelatine, and similar samples mixed with blood and then centrifuged. The calibration data have indicated that 51 Cr behaves anomalously, and its use as a label for microspheres may introduce unwarranted errors. A plane cylindrical 10 x 20 cm NaI detector was used, and a 'worst case' correction of 20% was found to be necessary for geometry effects. The accuracy of this method of correlating different geometries was tested by remodelling the same tissue sample into different sizes and comparing the results, and the validity of the technique was supported by agreement of the final results with previously published data. (U.K.)

  3. The use contrast agent for imaging biological samples

    Czech Academy of Sciences Publication Activity Database

    Dammer, J.; Weyda, František; Sopko, V.; Jakůbek, J.

    2011-01-01

    Roč. 6, C01096 (2011), s. 1-7 ISSN 1748-0221. [International Workshop on Radiation Imaging Detectors /12./. Cambridge, 11.07.2010-15.7.2010] R&D Projects: GA MŠk 2B06005 Grant - others:Research Program(CZ) 6840770029; Research Program(CZ) 6840770040; GA AV ČR(CZ) IAA600550614; GA MŠk(CZ) 2B06007; GA MŠk(CZ) 1PO4LA211; GA MŠk(CZ) LC06041 Program:IA; 2B; LC Institutional research plan: CEZ:AV0Z50070508 Keywords : x-ray radiography and digital radiography (DR) * x-ray detectors * inspections with x-rays Subject RIV: EA - Cell Biology Impact factor: 1.869, year: 2011

  4. Study of the spectral features of different biological samples

    Science.gov (United States)

    Atif, M.

    2015-03-01

    In the present study we have observed and analyzed the fluorescence changes in the fluorescence spectra of four different samples like brilliant sulphaflanine, quinine bisulphate, coumarine 120 and porcine cornea and sclera including the changes in fluorescence spectrum of cornea are also observed after CO2 laser exposure. The preliminary study clearly explains the proof of concept only.

  5. Cryogenic Collection of Complete Subsurface Samples for Molecular Biological Analysis

    Science.gov (United States)

    2012-05-01

    knowledge of indigenous microbial organisms, including their metabolic capabilities and the ways in which they respond to changing environmental... Indigenous Pseudomonas spp. in Soil Hot Spots. Applied and Environmental Microbiology, 65(4), 1786–1788. American Society for Microbiology. Retrieved...1428 856 0 96% 1 Environmental samples 1399 838 0 96% 1 Organism (phylum/ class/ genus ) Proteobacteria Uncultured Bacteria division OP11

  6. Soft Robotic Grippers for Biological Sampling on Deep Reefs.

    Science.gov (United States)

    Galloway, Kevin C; Becker, Kaitlyn P; Phillips, Brennan; Kirby, Jordan; Licht, Stephen; Tchernov, Dan; Wood, Robert J; Gruber, David F

    2016-03-01

    This article presents the development of an underwater gripper that utilizes soft robotics technology to delicately manipulate and sample fragile species on the deep reef. Existing solutions for deep sea robotic manipulation have historically been driven by the oil industry, resulting in destructive interactions with undersea life. Soft material robotics relies on compliant materials that are inherently impedance matched to natural environments and to soft or fragile organisms. We demonstrate design principles for soft robot end effectors, bench-top characterization of their grasping performance, and conclude by describing in situ testing at mesophotic depths. The result is the first use of soft robotics in the deep sea for the nondestructive sampling of benthic fauna.

  7. Adaptive optics for deeper imaging of biological samples.

    Science.gov (United States)

    Girkin, John M; Poland, Simon; Wright, Amanda J

    2009-02-01

    Optical microscopy has been a cornerstone of life science investigations since its first practical application around 400 years ago with the goal being subcellular resolution, three-dimensional images, at depth, in living samples. Nonlinear microscopy brought this dream a step closer, but as one images more deeply the material through which you image can greatly distort the view. By using optical devices, originally developed for astronomy, whose optical properties can be changed in real time, active compensation for sample-induced aberrations is possible. Submicron resolution images are now routinely recorded from depths over 1mm into tissue. Such active optical elements can also be used to keep conventional microscopes, both confocal and widefield, in optimal alignment.

  8. Mapping materials and biologic samples by scanning ionic microscopy

    International Nuclear Information System (INIS)

    Slodzian, G.

    1992-01-01

    In ionic microscopy images are obtained with atoms, from the object surface, sputtered by an ion beam. For each element, or isotope, the microscope gives an image and the illumination is proportional to the number of atoms of the element considered in the sample. Recent improvements increase the sensitivity, the spatial resolution and the superposition of ionic images from different elements of the same zone. Some examples are given

  9. Transuranium analysis methodologies for biological and environmental samples

    International Nuclear Information System (INIS)

    Wessman, R.A.; Lee, K.D.; Curry, B.; Leventhal, L.

    1978-01-01

    Analytical procedures for the most abundant transuranium nuclides in the environment (i.e., plutonium and, to a lesser extent, americium) are available. There is a lack of procedures for doing sequential analysis for Np, Pu, Am, and Cm in environmental samples, primarily because of current emphasis on Pu and Am. Reprocessing requirements and waste disposal connected with the fuel cycle indicate that neptunium and curium must be considered in environmental radioactive assessments. Therefore it was necessary to develop procedures that determine all four of these radionuclides in the environment. The state of the art of transuranium analysis methodology as applied to environmental samples is discussed relative to different sample sources, such as soil, vegetation, air, water, and animals. Isotope-dilution analysis with 243 Am ( 239 Np) and 236 Pu or 242 Pu radionuclide tracers is used. Americium and curium are analyzed as a group, with 243 Am as the tracer. Sequential extraction procedures employing bis(2-ethyl-hexyl)orthophosphoric acid (HDEHP) were found to result in lower yields and higher Am--Cm fractionation than ion-exchange methods

  10. Manipulation of nanoparticles and biological samples through enhanced optical forces

    Science.gov (United States)

    Wilson, Benjamin

    Non-invasive optical manipulation of particles has emerged as a powerful and versatile tool for biological study and nanotechnology. We propose and demonstrate large scale nanoparticle assembly using opto-thermal force produced by conventional optical tweezers. This method is shown to allow precise concentration and assembly of particles including carbon-nanotubes, VO2 nanorods, and CdTe quantum dots. Assembled devices were shown to have good contact with patterned electrodes. In addition, we propose and demonstrate a purely optical approach to rotate and align particles using the interaction of polarized light with photonic crystal nanostructures to generate enhanced trapping force. With a weakly focused laser beam we observed efficient trapping and transportation of polystyrene beads with sizes ranging from 10 microm down to 190 nm as well as cancer cell nuclei. In addition, we demonstrated alignment of non-spherical particles using a 1-D photonic crystal structure. Bacterial cells were trapped, rotated and aligned with optical intensity as low as 17 microW/microm 2. This approach can be extended to using 2-D photonic crystal nanostructures for full rotation control.

  11. Hexagonal ice in pure water and biological NMR samples

    Energy Technology Data Exchange (ETDEWEB)

    Bauer, Thomas; Gath, Julia; Hunkeler, Andreas; Ernst, Matthias, E-mail: maer@ethz.ch [ETH Zurich, Physical Chemistry (Switzerland); Böckmann, Anja, E-mail: a.bockmann@ibcp.fr [UMR 5086 CNRS, Université de Lyon 1, Institut de Biologie et Chimie des Protéines (France); Meier, Beat H., E-mail: beme@ethz.ch [ETH Zurich, Physical Chemistry (Switzerland)

    2017-01-15

    Ice, in addition to “liquid” water and protein, is an important component of protein samples for NMR spectroscopy at subfreezing temperatures but it has rarely been observed spectroscopically in this context. We characterize its spectroscopic behavior in the temperature range from 100 to 273 K, and find that it behaves like pure water ice. The interference of magic-angle spinning (MAS) as well as rf multiple-pulse sequences with Bjerrum-defect motion greatly influences the ice spectra.

  12. Elemental distribution and sample integrity comparison of freeze-dried and frozen-hydrated biological tissue samples with nuclear microprobe

    Energy Technology Data Exchange (ETDEWEB)

    Vavpetič, P., E-mail: primoz.vavpetic@ijs.si [Jožef Stefan Institute, Jamova 39, SI-1000 Ljubljana (Slovenia); Vogel-Mikuš, K. [Biotechnical Faculty, Department of Biology, University of Ljubljana, Jamnikarjeva 101, SI-1000 Ljubljana (Slovenia); Jeromel, L. [Jožef Stefan Institute, Jamova 39, SI-1000 Ljubljana (Slovenia); Ogrinc Potočnik, N. [Jožef Stefan Institute, Jamova 39, SI-1000 Ljubljana (Slovenia); FOM-Institute AMOLF, Science Park 104, 1098 XG Amsterdam (Netherlands); Pongrac, P. [Biotechnical Faculty, Department of Biology, University of Ljubljana, Jamnikarjeva 101, SI-1000 Ljubljana (Slovenia); Department of Plant Physiology, University of Bayreuth, Universitätstr. 30, 95447 Bayreuth (Germany); Drobne, D.; Pipan Tkalec, Ž.; Novak, S.; Kos, M.; Koren, Š.; Regvar, M. [Biotechnical Faculty, Department of Biology, University of Ljubljana, Jamnikarjeva 101, SI-1000 Ljubljana (Slovenia); Pelicon, P. [Jožef Stefan Institute, Jamova 39, SI-1000 Ljubljana (Slovenia)

    2015-04-01

    The analysis of biological samples in frozen-hydrated state with micro-PIXE technique at Jožef Stefan Institute (JSI) nuclear microprobe has matured to a point that enables us to measure and examine frozen tissue samples routinely as a standard research method. Cryotome-cut slice of frozen-hydrated biological sample is mounted between two thin foils and positioned on the sample holder. The temperature of the cold stage in the measuring chamber is kept below 130 K throughout the insertion of the samples and the proton beam exposure. Matrix composition of frozen-hydrated tissue is consisted mostly of ice. Sample deterioration during proton beam exposure is monitored during the experiment, as both Elastic Backscattering Spectrometry (EBS) and Scanning Transmission Ion Microscopy (STIM) in on–off axis geometry are recorded together with the events in two PIXE detectors and backscattered ions from the chopper in a single list-mode file. The aim of this experiment was to determine differences and similarities between two kinds of biological sample preparation techniques for micro-PIXE analysis, namely freeze-drying and frozen-hydrated sample preparation in order to evaluate the improvements in the elemental localisation of the latter technique if any. In the presented work, a standard micro-PIXE configuration for tissue mapping at JSI was used with five detection systems operating in parallel, with proton beam cross section of 1.0 × 1.0 μm{sup 2} and a beam current of 100 pA. The comparison of the resulting elemental distributions measured at the biological tissue prepared in the frozen-hydrated and in the freeze-dried state revealed differences in elemental distribution of particular elements at the cellular level due to the morphology alteration in particular tissue compartments induced either by water removal in the lyophilisation process or by unsatisfactory preparation of samples for cutting and mounting during the shock-freezing phase of sample preparation.

  13. Elemental distribution and sample integrity comparison of freeze-dried and frozen-hydrated biological tissue samples with nuclear microprobe

    International Nuclear Information System (INIS)

    Vavpetič, P.; Vogel-Mikuš, K.; Jeromel, L.; Ogrinc Potočnik, N.; Pongrac, P.; Drobne, D.; Pipan Tkalec, Ž.; Novak, S.; Kos, M.; Koren, Š.; Regvar, M.; Pelicon, P.

    2015-01-01

    The analysis of biological samples in frozen-hydrated state with micro-PIXE technique at Jožef Stefan Institute (JSI) nuclear microprobe has matured to a point that enables us to measure and examine frozen tissue samples routinely as a standard research method. Cryotome-cut slice of frozen-hydrated biological sample is mounted between two thin foils and positioned on the sample holder. The temperature of the cold stage in the measuring chamber is kept below 130 K throughout the insertion of the samples and the proton beam exposure. Matrix composition of frozen-hydrated tissue is consisted mostly of ice. Sample deterioration during proton beam exposure is monitored during the experiment, as both Elastic Backscattering Spectrometry (EBS) and Scanning Transmission Ion Microscopy (STIM) in on–off axis geometry are recorded together with the events in two PIXE detectors and backscattered ions from the chopper in a single list-mode file. The aim of this experiment was to determine differences and similarities between two kinds of biological sample preparation techniques for micro-PIXE analysis, namely freeze-drying and frozen-hydrated sample preparation in order to evaluate the improvements in the elemental localisation of the latter technique if any. In the presented work, a standard micro-PIXE configuration for tissue mapping at JSI was used with five detection systems operating in parallel, with proton beam cross section of 1.0 × 1.0 μm 2 and a beam current of 100 pA. The comparison of the resulting elemental distributions measured at the biological tissue prepared in the frozen-hydrated and in the freeze-dried state revealed differences in elemental distribution of particular elements at the cellular level due to the morphology alteration in particular tissue compartments induced either by water removal in the lyophilisation process or by unsatisfactory preparation of samples for cutting and mounting during the shock-freezing phase of sample preparation

  14. Unrealistic fatalism in U.S. youth ages 14 to 22: prevalence and characteristics.

    Science.gov (United States)

    Jamieson, Patrick E; Romer, Dan

    2008-02-01

    To estimate the proportion of U.S. youth that exhibits unrealistic fatalism about its future (not expecting to live past age 30), and to test predictions about risk factors for this expectation. Four waves of a nationally representative telephone survey from 2002 to 2005 with youth ages 14 to 22 (N = 4201) were analyzed using logistic regression to identify correlates and predictors of unrealistic fatalism. Approximately 1 out of every 15 youth interviewed (6.7%, 95% confidence interval [CI] = 5.9%, 7.5%) responded that they agreed they would not live much past the age of 30. Compared to other youth, fatalists were significantly more likely to be older, male, to identify as Hispanic, and have completed the interview in Spanish. As predicted, recent experience of hopelessness was a strong predictor of fatalism. In addition, nonwhite youth who had experienced hopelessness reported increasing rates of fatalism as they aged. Fatalistic youth engaged in greater suicidal planning, had more accepting attitudes toward suicide, were less attached to religion, and were more impulsive than other youth. Approximately 43% of fatalists forecast a likely death by suicide, whereas the rest anticipated death by an outside source. Fatalists were also more likely not to stay in school. Because youth exhibiting fatalism are at risk for not staying in school and suicidal planning, they should be identified at an early age for referral to programs that are effective in treating youth with hopelessness and suicidal tendencies.

  15. Standard reporting requirements for biological samples in metabolomics experiments: Microbial and in vitro biology experiments

    NARCIS (Netherlands)

    Werf, M.J. van der; Takors, R.; Smedsgaard, J.; Nielsen, J.; Ferenci, T.; Portais, J.C.; Wittmann, C.; Hooks, M.; Tomassini, A.; Oldiges, M.; Fostel, J.; Sauer, U.

    2007-01-01

    With the increasing use of metabolomics as a means to study a large number of different biological research questions, there is a need for a minimal set of reporting standards that allow the scientific community to evaluate, understand, repeat, compare and re-investigate metabolomics studies. Here

  16. Magnetic separation techniques in sample preparation for biological analysis: a review.

    Science.gov (United States)

    He, Jincan; Huang, Meiying; Wang, Dongmei; Zhang, Zhuomin; Li, Gongke

    2014-12-01

    Sample preparation is a fundamental and essential step in almost all the analytical procedures, especially for the analysis of complex samples like biological and environmental samples. In past decades, with advantages of superparamagnetic property, good biocompatibility and high binding capacity, functionalized magnetic materials have been widely applied in various processes of sample preparation for biological analysis. In this paper, the recent advancements of magnetic separation techniques based on magnetic materials in the field of sample preparation for biological analysis were reviewed. The strategy of magnetic separation techniques was summarized. The synthesis, stabilization and bio-functionalization of magnetic nanoparticles were reviewed in detail. Characterization of magnetic materials was also summarized. Moreover, the applications of magnetic separation techniques for the enrichment of protein, nucleic acid, cell, bioactive compound and immobilization of enzyme were described. Finally, the existed problems and possible trends of magnetic separation techniques for biological analysis in the future were proposed. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. [Mass spectrometry technology and its application in analysis of biological samples].

    Science.gov (United States)

    Zhao, Long-Shan; Li, Qing; Guo, Chao-Wei; Chen, Xiao-Hui; Bi, Kai-Shun

    2012-02-01

    With the excellent merits of wide analytical range, high sensitivity, small sample size, fast analysis speed, good repeatability, simple operation, low mobile phase consumption, as well as its capability of simultaneous isolation and identification, etc, mass spectrometry techniques have become widely used in the area of environmental science, energy chemical industry, biological medicine, and so on. This article reviews the application of mass spectrometry technology in biological sample analysis in the latest three years with the focus on the new applications in pharmacokinetics and bioequivalence, toxicokinetics, pharmacokinetic-pharmacodynamic, population pharmacokinetics, identification and fragmentation pathways of drugs and their metabolites and metabonomics to provide references for further study of biological sample analysis.

  18. Sample Preparation and Identification of Biological, Chemical and Mid-Spectrum Agents

    National Research Council Canada - National Science Library

    Hancock, J. R; Dragon, D. C

    2005-01-01

    A general survey of sample preparation and identification techniques for biological, chemical and mid-spectrum agents was conducted as part of Canada's contribution to a joint NATO Allied Engineering Publication (AEP) handbook...

  19. [Confirming Indicators of Qualitative Results by Chromatography-mass Spectrometry in Biological Samples].

    Science.gov (United States)

    Liu, S D; Zhang, D M; Zhang, W; Zhang, W F

    2017-04-01

    Because of the exist of complex matrix, the confirming indicators of qualitative results for toxic substances in biological samples by chromatography-mass spectrometry are different from that in non-biological samples. Even in biological samples, the confirming indicators are different in various application areas. This paper reviews the similarities and differences of confirming indicators for the analyte in biological samples by chromatography-mass spectrometry in the field of forensic toxicological analysis and other application areas. These confirming indicators include retention time (RT), relative retention time (RRT), signal to noise (S/N), characteristic ions, relative abundance of characteristic ions, parent ion-daughter ion pair and abundance ratio of ion pair, etc. Copyright© by the Editorial Department of Journal of Forensic Medicine.

  20. Robotic, MEMS-based Multi Utility Sample Preparation Instrument for ISS Biological Workstation, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — This project will develop a multi-functional, automated sample preparation instrument for biological wet-lab workstations on the ISS. The instrument is based on a...

  1. In modelling effects of global warming, invalid assumptions lead to unrealistic projections.

    Science.gov (United States)

    Lefevre, Sjannie; McKenzie, David J; Nilsson, Göran E

    2018-02-01

    In their recent Opinion, Pauly and Cheung () provide new projections of future maximum fish weight (W ∞ ). Based on criticism by Lefevre et al. (2017) they changed the scaling exponent for anabolism, d G . Here we find that changing both d G and the scaling exponent for catabolism, b, leads to the projection that fish may even become 98% smaller with a 1°C increase in temperature. This unrealistic outcome indicates that the current W ∞ is unlikely to be explained by the Gill-Oxygen Limitation Theory (GOLT) and, therefore, GOLT cannot be used as a mechanistic basis for model projections about fish size in a warmer world. © 2017 John Wiley & Sons Ltd.

  2. Dynamical 'in situ' observation of biological samples using variable pressure scanning electron microscope

    International Nuclear Information System (INIS)

    Nedela, V

    2008-01-01

    Possibilities of 'in-situ' observation of non-conductive biological samples free of charging artefacts in dynamically changed surrounding conditions are the topic of this work. The observed biological sample, the tongue of a rat, was placed on a cooled Peltier stage. We studied the visibility of topographical structure depending on transition between liquid and gas state of water in the specimen chamber of VP SEM.

  3. A Prototype Ice-Melting Probe for Collecting Biological Samples from Cryogenic Ice at Low Pressure.

    Science.gov (United States)

    Davis, Ashley

    2017-08-01

    In the Solar System, the surface of an icy moon is composed of irregular ice formations at cryogenic temperatures (mission, whose aim is to collect and analyze biological samples from the surface ice, must contain a device that collects samples without refreezing liquid and without sublimation of ice. In addition, if the samples are biological in nature, then precautions must be taken to ensure the samples do not overheat or mix with the oxidized layer. To achieve these conditions, the collector must maintain temperatures close to maintenance or growth conditions of the organism (moon-Microbe-Eukaryote-Spacecraft. Astrobiology 17, 709-720.

  4. Influence of sample collection and preanalytical sample processing on the analyses of biological markers in the European multicentre study IDEFICS.

    Science.gov (United States)

    Peplies, J; Günther, K; Bammann, K; Fraterman, A; Russo, P; Veidebaum, T; Tornaritis, M; Vanaelst, B; Mårild, S; Molnár, D; Moreno, L A; Ahrens, W

    2011-04-01

    To evaluate the influence of a standardised sampling protocol and process quality across the different IDEFICS (Identification and prevention of dietary- and lifestyle-induced health effects in children and infants) centres on the results of the biochemical measurements. Baseline survey within the community-based intervention study. A total of 16,224 children, aged 2-8 years, enrolled in the IDEFICS baseline survey in 8 European countries. Venous or capillary blood samples were collected from 12,430 children, urine samples from 13,890 children and saliva samples from 14,019 children. A set of quality indicators was recorded for the biological blood, urine and saliva samples collected during the IDEFICS study. Results of blood and urine measurements were analysed and stratified by selected quality indicators. Concentrations of biological markers in blood and urine measured during the IDEFICS baseline survey are associated with several quality indicators assessed in this study. Between-country variations of these biomarkers are described. It was confirmed that fasting has a big influence on the concentration of certain biomarkers. Biomarkers in morning urine samples may be erroneous if the study subjects void during the night or if samples are not taken from the very first morning urine. The analysed data underline that a standardised sampling protocol is of major importance, especially in multicentre studies, but non-compliance is ever present in spite of well-defined standard operation procedures. Deviations from the protocol should therefore always be documented to avoid error pertaining to the concentration of biological markers.

  5. Microfluidic devices for sample clean-up and screening of biological samples

    NARCIS (Netherlands)

    Tetala, K.K.R.

    2009-01-01

    Analytical chemistry plays an important role in the separation and identification of analytes from raw samples (e.g. plant extracts, blood), but the whole analytical process is tedious, difficult to automate and time consuming. To overcome these drawbacks, the concept of μTAS (miniaturized total

  6. Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

    OpenAIRE

    Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma; Abdel-Rehim, Mohamed

    2014-01-01

    In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from o...

  7. Determination of drugs in biological fluids by direct injection of samples for liquid-chromatographic analysis.

    Science.gov (United States)

    Mullett, Wayne M

    2007-03-10

    The analysis of drugs in various biological fluids is an important criterion for the determination of the physiological performance of a drug. After sampling of the biological fluid, the next step in the analytical process is sample preparation. The complexity of biological fluids adds to the challenge of direct determination of the drug by chromatographic analysis, therefore demanding a sample preparation step that is often time-consuming, tedious, and frequently overlooked. However, direct on-line injection methods offer the advantage of reducing sample preparation steps and enabling effective pre-concentration and clean-up of biological fluids. These procedures can be automated and therefore reduce the requirements for handling potentially infectious biomaterial, improve reproducibility, and minimize sample manipulations and potential contamination. The objective of this review is to present an overview of the existing literature with emphasis on advances in automated sample preparation methods for liquid-chromatographic methods. More specifically, this review concentrates on the use of direct injection techniques, such as restricted-access materials, turbulent-flow chromatography and other automated on-line solid-phase extraction (SPE) procedures. It also includes short overviews of emerging automated extraction-phase technologies, such as molecularly imprinted polymers, in-tube solid-phase micro-extraction, and micro-extraction in a packed syringe for a more selective extraction of analytes from complex samples, providing further improvements in the analysis of biological materials. Lastly, the outlook for these methods and potential new applications for these technologies are briefly discussed.

  8. Study of complex matrix effect on solid phase microextraction for biological sample analysis.

    Science.gov (United States)

    Jiang, Ruifen; Xu, Jianqiao; Zhu, Fang; Luan, Tiangang; Zeng, Feng; Shen, Yong; Ouyang, Gangfeng

    2015-09-11

    Solid phase microextraction (SPME) has become a useful tool for in vivo monitoring the behavior of environmental organic pollutants in biological species due to its simplicity, relatively non-invasive, and cost-effective manner. However, the complex matrices in biological samples could significantly influence the extraction kinetic, and bias the quantification result. In this study, we investigated the effect of complex matrix on the extraction kinetic of SPME for biological sample analysis. Two sample matrices, phosphate-buffered saline (PBS) with bovine serum albumin (BSA) and agarose gel with BSA were used to simulate the biological fluid and tissue. Results showed that the addition of BSA significantly enhanced the mass transfer of organic compounds onto SPME fiber in both PBS buffer and gel sample. Enhancement factors ranging from 1.3 to 27, and 2.0 to 80 were found for all selected polyaromatic hydrocarbons (PAHs) in PBS buffer and agarose gel with BSA concentration of 0.1-5%, respectively. Then, an improved theoretical model was applied to quantify the observed enhancement effect, and the result showed that the predicted sampling time constant agreed well with the experimental one in complex matrix. Furthermore, a simplified equation was proposed for the real biological sample analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Procedures for cryogenic X-ray ptychographic imaging of biological samples.

    Science.gov (United States)

    Yusuf, M; Zhang, F; Chen, B; Bhartiya, A; Cunnea, K; Wagner, U; Cacho-Nerin, F; Schwenke, J; Robinson, I K

    2017-03-01

    Biological sample-preparation procedures have been developed for imaging human chromosomes under cryogenic conditions. A new experimental setup, developed for imaging frozen samples using beamline I13 at Diamond Light Source, is described. This manuscript describes the equipment and experimental procedures as well as the authors' first ptychographic reconstructions using X-rays.

  10. Procedures for cryogenic X-ray ptychographic imaging of biological samples

    Directory of Open Access Journals (Sweden)

    M. Yusuf

    2017-03-01

    Full Text Available Biological sample-preparation procedures have been developed for imaging human chromosomes under cryogenic conditions. A new experimental setup, developed for imaging frozen samples using beamline I13 at Diamond Light Source, is described. This manuscript describes the equipment and experimental procedures as well as the authors' first ptychographic reconstructions using X-rays.

  11. Analysis of low-angle x-ray scattering peaks from lyophilized biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Desouky, Omar S. [Radiation Physics Department, National Center for Radiation Research and Technology, A.E.A., Cairo (Egypt)]. E-mail: omardesouky@yahoo.com; Elshemey, Wael M. [Biophysics Department, Faculty of Science, Cairo University (Egypt); Selim, Nabila S.; Ashour, Ahmed H. [Radiation Physics Department, National Center for Radiation Research and Technology, A.E.A., Cairo (Egypt)

    2001-08-01

    Low-angle x-ray scattering (LAXS) from lyophilized blood and its constituents is characterized by the presence of two peaks in the forward direction of scattering. These peaks are found to be sensitive to the variations in the molecular structure of a given sample. The present work aims to explore the nature of LAXS from a variety of lyophilized biological samples. It also aims to investigate the possibility that a certain biological macromolecule is responsible of the production of LAXS peaks. This is carried out through measurements of LAXS from complex biological samples and their basic constituents. Among the measured samples are haemoglobin (Hb), globin, haem, packed red blood cells, bovine albumin, egg albumin, milk, casein, glutamine, alanine, fat, muscle and DNA. A table containing some characteristic parameters of the LAXS profiles of these samples is also presented. Analysis of measured profiles shows that all lyophilized samples produce at least one relatively broad peak at a scattering angle around 10.35 deg. The full width at half maximum (FWHM) of this peak varies considerably among the measured samples. Except for milk and casein, one additional peak at a scattering angle around 4.65 deg. is observed only in the LAXS profiles of proteins or protein-rich samples. This fact strongly suggests protein to be the biological macromolecule from which this characteristic peak originates. The same idea is further strengthened through discussion of some previous observations. (author)

  12. Sample preparation strategies for food and biological samples prior to nanoparticle detection and imaging

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt; Löschner, Katrin

    2014-01-01

    Accurate and precise characterization of metrics such as size, mass, shape etc. of nanoparticles (NPs) remains a challenging task. In order to determine quantitative metrics that are relevant in food monitoring or in risk assessment, an instrumental separation method like asymmetric field flow...... fractionation (AFFF, or AF4) coupled on-line to various detectors including static and dynamic light scattering (LS), UV or fluorescence (FL) spectroscopies and ICP-MS have proven useful and powerful [1, 2, 3]. Furthermore, additional information obtained by an imaging method such as transmission electron...... for the meat sample extracts and the corresponding neat AgNP suspension, and rendered sizing by way of calibration with AgNPs as sizing standards inaccurate. In order to gain further insight into the sizes of the separated AgNPs, or their possible dissolved state, fractions of the AFFF eluate were collected...

  13. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    Directory of Open Access Journals (Sweden)

    Corina Mahu Ştefania

    2015-12-01

    Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

  14. Quantitating morphological changes in biological samples during scanning electron microscopy sample preparation with correlative super-resolution microscopy.

    Science.gov (United States)

    Zhang, Ying; Huang, Tao; Jorgens, Danielle M; Nickerson, Andrew; Lin, Li-Jung; Pelz, Joshua; Gray, Joe W; López, Claudia S; Nan, Xiaolin

    2017-01-01

    Sample preparation is critical to biological electron microscopy (EM), and there have been continuous efforts on optimizing the procedures to best preserve structures of interest in the sample. However, a quantitative characterization of the morphological changes associated with each step in EM sample preparation is currently lacking. Using correlative EM and superresolution microscopy (SRM), we have examined the effects of different drying methods as well as osmium tetroxide (OsO4) post-fixation on cell morphology during scanning electron microscopy (SEM) sample preparation. Here, SRM images of the sample acquired under hydrated conditions were used as a baseline for evaluating morphological changes as the sample went through SEM sample processing. We found that both chemical drying and critical point drying lead to a mild cellular boundary retraction of ~60 nm. Post-fixation by OsO4 causes at least 40 nm additional boundary retraction. We also found that coating coverslips with adhesion molecules such as fibronectin prior to cell plating helps reduce cell distortion from OsO4 post-fixation. These quantitative measurements offer useful information for identifying causes of cell distortions in SEM sample preparation and improving current procedures.

  15. Electromembrane extraction as a rapid and selective miniaturized sample preparation technique for biological fluids

    DEFF Research Database (Denmark)

    Gjelstad, Astrid; Pedersen-Bjergaard, Stig; Seip, Knut Fredrik

    2015-01-01

    This special report discusses the sample preparation method electromembrane extraction, which was introduced in 2006 as a rapid and selective miniaturized extraction method. The extraction principle is based on isolation of charged analytes extracted from an aqueous sample, across a thin film....... Technical aspects of electromembrane extraction, important extraction parameters as well as a handful of examples of applications from different biological samples and bioanalytical areas are discussed in the paper....

  16. Standard operating procedure for combustion of 14C - samples with OX-500 biological material oxidizer

    International Nuclear Information System (INIS)

    Nashriyah Mat.

    1995-01-01

    This procedure is for the purpose of safe operation of OX-500 biological material oxidizer. For ease of operation, the operation flow chart (including testing the system and sample combustion) and end of day maintenance flow chart were simplified. The front view, diagrams and switches are duly copied from operating manual. Steps on sample preparation are also included for biotic and a biotic samples. This operating procedure is subjected to future reviews

  17. Chemometric and Statistical Analyses of ToF-SIMS Spectra of Increasingly Complex Biological Samples

    Energy Technology Data Exchange (ETDEWEB)

    Berman, E S; Wu, L; Fortson, S L; Nelson, D O; Kulp, K S; Wu, K J

    2007-10-24

    Characterizing and classifying molecular variation within biological samples is critical for determining fundamental mechanisms of biological processes that will lead to new insights including improved disease understanding. Towards these ends, time-of-flight secondary ion mass spectrometry (ToF-SIMS) was used to examine increasingly complex samples of biological relevance, including monosaccharide isomers, pure proteins, complex protein mixtures, and mouse embryo tissues. The complex mass spectral data sets produced were analyzed using five common statistical and chemometric multivariate analysis techniques: principal component analysis (PCA), linear discriminant analysis (LDA), partial least squares discriminant analysis (PLSDA), soft independent modeling of class analogy (SIMCA), and decision tree analysis by recursive partitioning. PCA was found to be a valuable first step in multivariate analysis, providing insight both into the relative groupings of samples and into the molecular basis for those groupings. For the monosaccharides, pure proteins and protein mixture samples, all of LDA, PLSDA, and SIMCA were found to produce excellent classification given a sufficient number of compound variables calculated. For the mouse embryo tissues, however, SIMCA did not produce as accurate a classification. The decision tree analysis was found to be the least successful for all the data sets, providing neither as accurate a classification nor chemical insight for any of the tested samples. Based on these results we conclude that as the complexity of the sample increases, so must the sophistication of the multivariate technique used to classify the samples. PCA is a preferred first step for understanding ToF-SIMS data that can be followed by either LDA or PLSDA for effective classification analysis. This study demonstrates the strength of ToF-SIMS combined with multivariate statistical and chemometric techniques to classify increasingly complex biological samples

  18. Presence of pesticide residues in water, sediment and biological samples taken from aquatic environments in Honduras

    International Nuclear Information System (INIS)

    Meyer, D.E.

    1999-01-01

    The objective of this study was to detect the presence of persistent pesticides in water, sediment and biological samples taken from aquatic environments in Honduras during the period 1995-98. Additionally, the LC 50 for 2 fungicides and 2 insecticides on post-larval Penaeus vannamei was determined in static water bioassays. A total of 80 water samples, 16 sediment samples and 7 biological samples (fish muscle tissue) were analyzed for detection of organochlorine and organophosphate pesticide residues. The results of sample analyses indicate a widespread contamination of Honduran continental and coastal waters with organochlorine pesticides. Most detections were of low ( 50 values and were therefore found to be much more toxic to the post-larval shrimp than the fungicides tridemorph and propiconazole. (author)

  19. On the accuracy of protein determination in large biological samples by prompt gamma neutron activation analysis

    International Nuclear Information System (INIS)

    Kasviki, K.; Stamatelatos, I.E.; Yannakopoulou, E.; Papadopoulou, P.; Kalef-Ezra, J.

    2007-01-01

    A prompt gamma neutron activation analysis (PGNAA) facility has been developed for the determination of nitrogen and thus total protein in large volume biological samples or the whole body of small animals. In the present work, the accuracy of nitrogen determination by PGNAA in phantoms of known composition as well as in four raw ground meat samples of about 1 kg mass was examined. Dumas combustion and Kjeldahl techniques were also used for the assessment of nitrogen concentration in the meat samples. No statistically significant differences were found between the concentrations assessed by the three techniques. The results of this work demonstrate the applicability of PGNAA for the assessment of total protein in biological samples of 0.25-1.5 kg mass, such as a meat sample or the body of small animal even in vivo with an equivalent radiation dose of about 40 mSv

  20. Energy-filtered transmission electron microscopy of biological samples on highly transparent carbon nanomembranes

    International Nuclear Information System (INIS)

    Rhinow, Daniel; Bueenfeld, Matthias; Weber, Nils-Eike; Beyer, Andre; Goelzhaeuser, Armin; Kuehlbrandt, Werner; Hampp, Norbert; Turchanin, Andrey

    2011-01-01

    Ultrathin carbon nanomembranes (CNM) comprising crosslinked biphenyl precursors have been tested as support films for energy-filtered transmission electron microscopy (EFTEM) of biological specimens. Due to their high transparency CNM are ideal substrates for electron energy loss spectroscopy (EELS) and electron spectroscopic imaging (ESI) of stained and unstained biological samples. Virtually background-free elemental maps of tobacco mosaic virus (TMV) and ferritin have been obtained from samples supported by ∼1 nm thin CNM. Furthermore, we have tested conductive carbon nanomembranes (cCNM) comprising nanocrystalline graphene, obtained by thermal treatment of CNM, as supports for cryoEM of ice-embedded biological samples. We imaged ice-embedded TMV on cCNM and compared the results with images of ice-embedded TMV on conventional carbon film (CC), thus analyzing the gain in contrast for TMV on cCNM in a quantitative manner. In addition we have developed a method for the preparation of vitrified specimens, suspended over the holes of a conventional holey carbon film, while backed by ultrathin cCNM. -- Research highlights: → We examine ultrathin carbon nanomembranes (CNM) as supports for biological TEM. → CNM comprise crosslinked biphenyl precursors. → CNM supports enable background-free elemental mapping of heavy and light elements. → We perform cryoEM of ice-embedded biological samples on graphene-like conductive CNM.

  1. Quantitative HPLC determination of [99mTc]-pertechnetate in radiopharmaceuticals and biological samples: Pt. 1

    International Nuclear Information System (INIS)

    Tianze Zhou; Hirth, W.W.; Heineman, W.R.; Deutsch, Edward

    1988-01-01

    Techniques have been developed which allow HPLC (high performance liquid chromatography) to be used for the quantitative determination of [ 99m Tc]pertechnetate in radiopharmaceuticals and biological samples. An instrumental technique accounts for 99m Tc species which do not elute from the HPLC column, while a chemical technique obviates interferences caused by Sn(II). These two techniques are incorporated into an anion exchange HPLC procedure which is applied to the determination of [ 99m Tc]pertechnetate in 99m Tc-diphosphonate radiopharmaceuticals and biological samples. (author)

  2. High resolution computational on-chip imaging of biological samples using sparsity constraint (Conference Presentation)

    Science.gov (United States)

    Rivenson, Yair; Wu, Chris; Wang, Hongda; Zhang, Yibo; Ozcan, Aydogan

    2017-03-01

    Microscopic imaging of biological samples such as pathology slides is one of the standard diagnostic methods for screening various diseases, including cancer. These biological samples are usually imaged using traditional optical microscopy tools; however, the high cost, bulkiness and limited imaging throughput of traditional microscopes partially restrict their deployment in resource-limited settings. In order to mitigate this, we previously demonstrated a cost-effective and compact lens-less on-chip microscopy platform with a wide field-of-view of >20-30 mm^2. The lens-less microscopy platform has shown its effectiveness for imaging of highly connected biological samples, such as pathology slides of various tissue samples and smears, among others. This computational holographic microscope requires a set of super-resolved holograms acquired at multiple sample-to-sensor distances, which are used as input to an iterative phase recovery algorithm and holographic reconstruction process, yielding high-resolution images of the samples in phase and amplitude channels. Here we demonstrate that in order to reconstruct clinically relevant images with high resolution and image contrast, we require less than 50% of the previously reported nominal number of holograms acquired at different sample-to-sensor distances. This is achieved by incorporating a loose sparsity constraint as part of the iterative holographic object reconstruction. We demonstrate the success of this sparsity-based computational lens-less microscopy platform by imaging pathology slides of breast cancer tissue and Papanicolaou (Pap) smears.

  3. On multielement analysis of biological samples with the aid of neutron activation

    International Nuclear Information System (INIS)

    Iyengar, G.V.

    1980-01-01

    A main objective of this study was elucidation of problems of sampling and sample preparation methods for multielement analysis of environmental and biological specimens. Another was assessment of the potentials of multielement neutron activation analysis (NAA) in environmental and biological research. In an attempt to explain the great differences in the elemental concentration ranges between biopsy and autopsy samples as reported in the literature, it was shown that post mortem changes induce great variations in the apparent elemental composition of autopsy specimens resulting in serious systematic errors. Applications of NAA to analysis of tissues of experimental animals, human tissues in health and disease, and environmental samples are illustrated with several examples. The suitability of NAA for routine analysis of elements such as Cr, Mo and Se, which are difficult to determine by other methods has been specially discussed. (author)

  4. Method for the concentration and separation of actinides from biological and environmental samples

    Science.gov (United States)

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

    1989-05-30

    A method and apparatus for the quantitative recover of actinide values from biological and environmental sample by passing appropriately prepared samples in a mineral acid solution through a separation column of a dialkyl(phenyl)-N,N-dialylcarbamoylmethylphosphine oxide dissolved in tri-n-butyl phosphate on an inert substrate which selectively extracts the actinide values. The actinide values can be eluted either as a group or individually and their presence quantitatively detected by alpha counting. 3 figs.

  5. Losses of some elements during dry ashing of marine biological samples

    International Nuclear Information System (INIS)

    Kawashima, Tatsuro; Koda, Yoshio; Yamamoto, Toshio.

    1982-01-01

    The losses of elements in marine biological samples during dry ashing were evaluated on 34 elements by neutron activation analysis. Following biological samples were employed: Eisenia bicyclis (phacophyceae), Sargassum tortile (phaeophyceae), Zostera marina (phanerogamae), small dried sardines (marine fish), and leaves of Crinum asiaticum (angiospermae). Before ashing, samples were freeze-crushed with liquid nitrogen. These samples were ashed at 100 0 C in low temperature plasma ashing and at 500 0 C in high temperature ashing. Both the dried and the ashed samples were irradiated simultaneously by thermal neutrons of a KUR reactor for activation analysis. Radioactivity measurements were carried out with a 63 cm 3 well type Ge(Li) detector and a Canberra-2048 channel pulse-height analyser over one year after the irradiation. Chlorine, arsenic, selenium, bromine, iodine, gold, and mercury were obviously lost during high temperature ashing. Low temperature plasma ashing was effective for reducing the losses of arsenic and selenium. Depending on the kind of biological samples, there were remarkable differences in losses of halogen elements. (author)

  6. Controlled dehydration of a biological sample using an alternative form of environmental SEM

    Czech Academy of Sciences Publication Activity Database

    Neděla, Vilém

    2010-01-01

    Roč. 237, č. 1 (2010), s. 7-11 ISSN 0022-2720 Institutional research plan: CEZ:AV0Z20650511 Keywords : biological sample * dehydration * environmental SEM * AQUASEM II * hydration system Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.872, year: 2010

  7. Evaluation of Botanical Reference Materials for the Determination of Vanadium in Biological Samples

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Damsgaard, Else

    1982-01-01

    Three botanical reference materials prepared by the National Bureau of Standards have been studied by neutron activation analysis to evaluate their suitability with respect to the determination of vanadium in biological samples. Various decomposition methods were applied in connection with chemical...

  8. MCT-based SWIR hyperspectral imaging system for evaluation of biological samples

    Science.gov (United States)

    Hyperspectral imaging has been shown to be a powerful tool for nondestructive evaluation of biological samples. We recently developed a new line-scan-based shortwave infrared (SWIR) hyperspectral imaging system. Critical sensing components of the system include a SWIR spectrograph, an MCT (HgCdTe) a...

  9. Biological sample evaluation using a line-scan based SWIR hyperspectral imaging system

    Science.gov (United States)

    A new line-scan hyperspectral imaging system was developed to enable short wavelength infrared (SWIR) imagery for biological sample evaluation. Critical sensing components include a SWIR imaging spectrograph and an HgCdTe (MCT) focal plane array detector. To date, agricultural applications of infra...

  10. Micro-electromembrane extraction across free liquid membranes. Extractions of basic drugs from undiluted biological samples

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2014-01-01

    Roč. 1337, Apr (2014), s. 32-39 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : micro-electromembrane extraction * free liquid membranes * biological samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 4.169, year: 2014

  11. Micro-electromembrane extraction across free liquid membranes. Extractions of basic drugs from undiluted biological samples

    Czech Academy of Sciences Publication Activity Database

    Kubáň, Pavel; Boček, Petr

    2014-01-01

    Roč. 1337, Apr (2014), s. 32-39 ISSN 0021-9673 R&D Projects: GA ČR(CZ) GA13-05762S Institutional support: RVO:68081715 Keywords : micro-electromembrane extraction * free liquid membranes * biological samples Subject RIV: CB - Analytical Chemistry , Separation Impact factor: 4.169, year: 2014

  12. Phytochemical analysis and biological evaluation of selected African propolis samples from Cameroon and Congo

    NARCIS (Netherlands)

    Papachroni, D.; Graikou, K.; Kosalec, I.; Damianakos, H.; Ingram, V.J.; Chinou, I.

    2015-01-01

    The objective of this study was the chemical analysis of four selected samples of African propolis (Congo and Cameroon) and their biological evaluation. Twenty-one secondary metabolites belonging to four different chemical groups were isolated from the 70% ethanolic extracts of propolis and their

  13. Sample preparation for liquid chromatographic analysis of phytochemicals in biological fluids.

    Science.gov (United States)

    Oh, Ju-Hee; Lee, Young-Joo

    2014-01-01

    Natural products have been used traditionally for the treatment and prevention of diseases for thousands of years and are nowadays consumed as dietary supplements and herbal medicine. To ensure the safe and effective use of these herbal products, information about bioavailability of active compounds in plasma or target tissues should be provided via validated analytical methods combined with appropriate sampling methods. To provide comprehensive and abridged information about sample preparation methods for the quantification of phytochemicals in biological samples using liquid chromatography analysis. Sample pre-treatment procedures used in analytical methods for in vivo pharmacokinetic studies of natural compounds or herbal medicines were reviewed. These were categorised according to the biological matrices (plasma, bile, urine, faeces and tissues) and sample clean-up processes (protein precipitation, liquid-liquid extraction and solid-phase extraction). Although various kinds of sample pre-treatment methods have been developed, liquid-liquid extraction is still widely used and solid-phase extraction is becoming increasingly popular because of its efficiency for extensive clean up of complex matrix samples. However, protein precipitation is still favoured due to its simplicity. Sample treatment for phytochemical analysis in biological fluids is an indispensable and critical step to obtain high quality results. This step could dominate the overall analytical process because both the duration of the process as well as the reliability of the data depend in large part on its efficiency. Thus, special attention should be given to the choice of a proper sample treatment method that targets analytes and their biomatrix. Copyright © 2013 John Wiley & Sons, Ltd.

  14. Toward greener analytical techniques for the absolute quantification of peptides in pharmaceutical and biological samples.

    Science.gov (United States)

    Van Eeckhaut, Ann; Mangelings, Debby

    2015-09-10

    Peptide-based biopharmaceuticals represent one of the fastest growing classes of new drug molecules. New reaction types included in the synthesis strategies to reduce the rapid metabolism of peptides, along with the availability of new formulation and delivery technologies, resulted in an increased marketing of peptide drug products. In this regard, the development of analytical methods for quantification of peptides in pharmaceutical and biological samples is of utmost importance. From the sample preparation step to their analysis by means of chromatographic or electrophoretic methods, many difficulties should be tackled to analyze them. Recent developments in analytical techniques emphasize more and more on the use of green analytical techniques. This review will discuss the progresses in and challenges observed during green analytical method development for the quantification of peptides in pharmaceutical and biological samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  15. A Method for Determining the Content of Glycoproteins in Biological Samples

    Directory of Open Access Journals (Sweden)

    Yang Gao

    2016-11-01

    Full Text Available The glycoprotein purified from the mycelium extract of Tremella fuciformis was marked with iodine through the iodine substitution reaction. The content of iodine, which is indicative of the amount of the marked tremella glycoprotein (ITG, was detected with Inductively coupled plasma mass spectrometry (ICP-MS. The method was found to be stable, sensitive, and accurate at detecting the content of iodine-substituted glycoprotein, and was used in the quantitative analysis of biological samples, including blood and organs. Different biological samples were collected from rats after oral administration of ITG, and were tested for iodine content by ICP-MS to calculate the amount of ITG in the samples. The results suggested that ICP-MS is a sensitive, stable, and accurate method for detection of iodinated glycoproteins in blood and organs.

  16. Improved methods for generation, sampling, and recovery of biological aerosols in filter challenge tests.

    Science.gov (United States)

    McCullough, N V; Brosseau, L M; Vesley, D; Vincent, J H

    1998-04-01

    In preparation for filter efficiency tests and sampler comparison studies, methods of biological aerosol generation, sampling, and filter recovery were modified from previous studies. Methods described include (1) techniques for generating aerosols that reduced nuisance particles to negligible levels and increased the cell culturability of Mycobacterium abscessus by 30%, (2) sampling techniques that lowered the detectable range of biological particle size from 0.65 to 0.45 micron and reduced the sampling flow from the chamber from 28.3 to 1.5 L/min, and (3) development of methods to remove culturable organisms from respirator filter media. These methods were developed for filter challenge tests with M. abscessus and were applied to two other bacteria. They may also have application to a wider variety of organisms and bioaerosol assessments.

  17. Advantages of infrared transflection micro spectroscopy and paraffin-embedded sample preparation for biological studies

    Science.gov (United States)

    Yao, Jie; Li, Qian; Zhou, Bo; Wang, Dan; Wu, Rie

    2018-04-01

    Fourier-Transform Infrared micro-spectroscopy is an excellent method for biological analyses. In this paper, series metal coating films on ITO glass were prepared by the electrochemical method and the different thicknesses of paraffin embedding rat's brain tissue on the substrates were studied by IR micro-spetroscopy in attenuated total reflection (ATR) mode and transflection mode respectively. The Co-Ni-Cu alloy coating film with low cost is good reflection substrates for the IR analysis. The infrared microscopic transflection mode needs not to touch the sample at all and can get the IR spectra with higher signal to noise ratios. The Paraffin-embedding method allows tissues to be stored for a long time for re-analysis to ensure the traceability of the sample. Also it isolates the sample from the metal and avoids the interaction of biological tissue with the metals. The best thickness of the tissues is 4 μm.

  18. Direct observation of unstained wet biological samples by scanning-electron generation X-ray microscopy

    International Nuclear Information System (INIS)

    Ogura, Toshihiko

    2010-01-01

    Analytical tools of nanometre-scale resolution are indispensable in the fields of biology, physics and chemistry. One suitable tool, the soft X-ray microscope, provides high spatial resolution of visible light for wet specimens. For biological specimens, X-rays of water-window wavelength between carbon (284 eV; 4.3 nm) and oxygen (540 eV; 2.3 nm) absorption edges provide high-contrast imaging of biological samples in water. Among types of X-ray microscope, the transmission X-ray microscope using a synchrotron radiation source with diffractive zone plates offers the highest spatial resolution, approaching 15-10 nm. However, even higher resolution is required to measure proteins and protein complexes in biological specimens; therefore, a new type of X-ray microscope with higher resolution that uses a simple light source is desirable. Here we report a novel scanning-electron generation X-ray microscope (SGXM) that demonstrates direct imaging of unstained wet biological specimens. We deposited wet yeasts in the space between two silicon nitride (Si 3 N 4 ) films. A scanning electron beam of accelerating voltage 5 keV and current 1.6 nA irradiates the titanium (Ti)-coated Si 3 N 4 film, and the soft X-ray signal from it is detected by an X-ray photodiode (PD) placed below the sample. The SGXM can theoretically achieve better than 5 nm resolution. Our method can be utilized easily for various wet biological samples of bacteria, viruses, and protein complexes.

  19. Inductively coupled plasma mass spectrometry in the analysis of biological samples and pharmaceutical drugs

    Science.gov (United States)

    Ossipov, K.; Seregina, I. F.; Bolshov, M. A.

    2016-04-01

    Inductively coupled plasma mass spectrometry (ICP-MS) is widely used in the analysis of biological samples (whole blood, serum, blood plasma, urine, tissues, etc.) and pharmaceutical drugs. The shortcomings of this method related to spectral and non-spectral interferences are manifested in full measure in determination of the target analytes in these complex samples strongly differing in composition. The spectral interferences are caused by similarity of masses of the target component and sample matrix components. Non-spectral interferences are related to the influence of sample matrix components on the physicochemical processes taking place during formation and transportation of liquid sample aerosols into the plasma, on the value and spatial distribution of plasma temperature and on the transmission of the ion beam from the interface to mass spectrometer detector. The review is devoted to analysis of different mechanisms of appearance of non-spectral interferences and to ways for their minimization or elimination. Special attention is paid to the techniques of biological sample preparation, which largely determine the mechanisms of the influence of sample composition on the results of element determination. The ways of lowering non-spectral interferences by instrumental parameter tuning and application of internal standards are considered. The bibliography includes 189 references.

  20. Will Women Diagnosed with Breast Cancer Provide Biological Samples for Research Purposes?

    Directory of Open Access Journals (Sweden)

    Shelley A Harris

    Full Text Available Little is known about the response rates for biological sample donation and attitudes towards control recruitment, especially in younger women. The goals of this pilot study were to determine in women recently diagnosed with breast cancer, the proportion of cases willing to provide biological samples and for purposes of control recruitment, contact information for friends or colleagues.A population-based sample of breast cancer cases (n = 417, 25-74 years was recruited from the Ontario Cancer Registry in 2010 and self-administered questionnaires were completed to determine willingness to provide samples (spot or 24-hr urine, saliva, blood and contact information for friends/colleagues for control recruitment. Using Χ2 analyses of contingency tables we evaluated if these proportions varied by age group (<45 and 45+ and other factors such as ethnicity, education, income, body mass index (BMI, smoking status and alcohol consumption.Cases were willing to provide blood samples, by visiting a clinic (62% or by having a nurse visit the home (61%. Moreover, they would provide saliva (73%, and morning or 24-hr urine samples (66% and 52%. Younger cases (≤45 were 3 times (OR more likely more than older cases to agree to collect morning urine (95% CI: 1.15-8.35. Only 26% of cases indicated they would provide contact information of friends or work colleagues to act as controls. Educated cases were more likely to agree to provide samples, and cases who consumed alcohol were more willing to provide contact information. Ethnicity, income, BMI and smoking had little effect on response rates.Reasonable response rates for biological sample collection should be expected in future case controls studies in younger women, but other methods of control selection must be devised.

  1. [Experience with a rheumatoid arthritis biobank: analysis of biological samples and clinical data of 204 patients].

    Science.gov (United States)

    Pál, Ildikó; Pusztai, Anita; Csomor, Péter; Szekanecz, Zoltán

    2017-02-01

    A biobank is a registry, which is suitable for the storage of biological samples (e.g. tissues, DNA, protein), genetical abnormalities and clinical data. Several biobanks have been created worldwide, which contribute to research and the better understanding of disease pathogenesis, genetical polymorphisms. Biobanking also helps to improve the efficacy of therapies. Our purpose was to create an internet-based biobank, in which laboratory test results, genetic alterations and related disorders of rheumatoid arthritis (RA) patients can be registered. This biobank would be able to make the research easier and it can help to improve our knowledge about diseases and it can inhibit loss of data. We have biological samples from 204 RA patients and we have entered their data in the biobank which can be found on the website http://rheuma.biobank.eu . Statistical analysis was performed by SPSS20 statistical programme. By the creation of biobank that contains clinical data and biological samples of 204 RA patients, we have a database which can help to improve our knowledge about the disease and help to develop new treatment strategies. Biobanking is suitable to analyze blood samples and clinical data together. Orv. Hetil., 2017, 158(7), 270-277.

  2. Hyperspectral imaging of nanoparticles in biological samples: Simultaneous visualization and elemental identification.

    Science.gov (United States)

    Peña, María Del Pilar Sosa; Gottipati, Abhishek; Tahiliani, Sahil; Neu-Baker, Nicole M; Frame, Mary D; Friedman, Adam J; Brenner, Sara A

    2016-05-01

    While engineered nanomaterials (ENMs) are increasingly incorporated into industrial processes and consumer products, the potential biological effects and health outcomes of exposure remain unknown. Novel advanced direct visualization techniques that require less time, cost, and resource investment than electron microscopy (EM) are needed for identifying and locating ENMs in biological samples. Hyperspectral imaging (HSI) combines spectrophotometry and imaging, using advanced optics and algorithms to capture a spectrum from 400 to 1000 nm at each pixel in an enhanced dark-field microscopic (EDFM) image. HSI-EDFM can be used to confirm the identity of the materials of interest in a sample and generate an image "mapping" their presence and location in a sample. Hyperspectral mapping is particularly important for biological samples, where ENM morphology is visually indistinct from surrounding tissue structures. While use of HSI (without mapping) is increasing, no studies to date have compared results from hyperspectral mapping with conventional methods. Thus, the objective of this study was to utilize EDFM-HSI to locate, identify, and map metal oxide ENMs in ex vivo histological porcine skin tissues, a toxicological model of cutaneous exposure, and compare findings with those of Raman spectroscopy (RS), energy-dispersive X-ray spectroscopy (EDS), and scanning electron microscopy (SEM). Results demonstrate that EDFM-HSI mapping is capable of locating and identifying ENMs in tissue, as confirmed by conventional methods. This study serves as initial confirmation of EDFM-HSI mapping as a novel and higher throughput technique for ENM identification in biological samples, and serves as the basis for further protocol development utilizing EDFM-HSI for semiquantitation of ENMs. © 2016 Wiley Periodicals, Inc.

  3. Elemental and isotopic imaging of biological samples using NanoSIMS.

    Science.gov (United States)

    Kilburn, Matt R; Clode, Peta L

    2014-01-01

    With its low detection limits and the ability to analyze most of the elements in the periodic table, secondary ion mass spectrometry (SIMS) represents one of the most versatile in situ analytical techniques available, and recent developments have resulted in significant advantages for the use of imaging mass spectrometry in biological and biomedical research. Increases in spatial resolution and sensitivity allow detailed interrogation of samples at relevant scales and chemical concentrations. Advances in dynamic SIMS, specifically with the advent of NanoSIMS, now allow the tracking of stable isotopes within biological systems at subcellular length scales, while static SIMS combines subcellular imaging with molecular identification. In this chapter, we present an introduction to the SIMS technique, with particular reference to NanoSIMS, and discuss its application in biological and biomedical research.

  4. Axial-scanning low-coherence interferometer method for noncontact thickness measurement of biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Do-Hyun; Song, Chul-Gyu; Ilev, Ilko K.; Kang, Jin U.

    2011-02-20

    We investigated a high-precision optical method for measuring the thickness of biological samples regardless of their transparency. The method is based on the precise measurement of optical path length difference of the end surfaces of objects, using a dual-arm axial-scanning low-coherence interferometer. This removes any consideration of the shape, thickness, or transparency of testing objects when performing the measurement. Scanning the reference simplifies the measurement setup, resulting in unambiguous measurement. Using a 1310 nm wavelength superluminescent diode, with a 65 nm bandwidth, the measurement accuracy was as high as 11.6 {mu}m. We tested the method by measuring the thickness of both transparent samples and nontransparent soft biological tissues.

  5. Specific determination of clinical and toxicological important substances in biological samples by LC-MS

    International Nuclear Information System (INIS)

    Mitulovic, G.

    2001-02-01

    This thesis of this dissertation is the specific determination of clinical and toxicological important substances in biological samples by LC-MS. Nicotine was determined in serum after application of nicotine plaster and nicotine nasal spray with HPLC-ESI-MS. Cotinine was determined direct in urine with HPLC-ESI-MS. Short time anesthetics were determined in blood and cytostatics were determined in liquor with HPLC-ESI-MS. (botek)

  6. Dynamical "in situ" observation of biological samples using variable pressure scanning electron microscope

    Czech Academy of Sciences Publication Activity Database

    Neděla, Vilém

    2008-01-01

    Roč. 126, - (2008), 012046:1-4 ISSN 1742-6588. [Electron Microscopy and Analysis Group Conference 2007 (EMAG 2007). Glasgow, 03.09.2007-07.09.2007] R&D Projects: GA ČR(CZ) GA102/05/0886; GA AV ČR KJB200650602 Institutional research plan: CEZ:AV0Z20650511 Keywords : biological sample * VP-SEM * dynamical experiments Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering

  7. A comparative examination of sample treatment procedures for ICAP-AES analysis of biological tissue

    Science.gov (United States)

    De Boer, J. L. M.; Maessen, F. J. M. J.

    The objective of this study was to contribute to the evaluation of existing sample preparation procedures for ICAP-AES analysis of biological material. Performance characteristics were established of current digestion procedures comprising extraction, solubilization, pressure digestion, and wet and dry ashing methods. Apart from accuracy and precision, a number of criteria of special interest for the analytical practice was applied. As a test sample served SRM bovine liver. In this material six elements were simultaneously determined. Results showed that every procedure has its defects and advantages. Hence, unambiguous recommendation of standard digestion procedures can be made only when taking into account the specific analytical problem.

  8. Ultrasensitive Hybridization-Based ELISA Method for the Determination of Phosphorodiamidate Morpholino Oligonucleotides in Biological samples.

    Science.gov (United States)

    Burki, Umar; Straub, Volker

    2017-01-01

    Determining the concentration of oligonucleotide in biological samples such as tissue lysate and serum is essential for determining the biodistribution and pharmacokinetic profile, respectively. ELISA-based assays have shown far greater sensitivities compared to other methods such as HPLC and LC/MS. Here, we describe a novel ultrasensitive hybridization-based ELISA method for quantitating morpholino oligonucleotides in mouse tissue lysate and serum samples. The assay has a linear detection range of 5-250 pM (R2 > 0.99).

  9. Determination of phosphorus in biological samples by thermal neutron activation followed by β--counting

    International Nuclear Information System (INIS)

    Weginwar, R.G.; Samudralwar, D.L.; Garg, A.N.

    1989-01-01

    Phosphorus was determined using the β - emitter 32 P by instrumental neutron activation analysis (INAA) in several NBS and IAEA standards, and in samples of biological origin such as human and animal blood, cancerous tissue, edible plant leaves, diets, milk samples, etc. The method involves thermal neutron irradiation (for 2-10 h in a reactor) followed by β - counting on an end-window gas flow proportional counter using aluminium filter. The results are within ±10% of the certified values in most cases. (author) 29 refs.; 3 tabs

  10. Convergent synthesis of a deuterium-labeled serine dipeptide lipid for analysis of biological samples.

    Science.gov (United States)

    Dietz, Christopher; Clark, Robert B; Nichols, Frank C; Smith, Michael B

    2017-05-30

    Bacterial serine dipeptide lipids are known to promote inflammatory processes and are detected in human tissues associated with periodontal disease or atherosclerosis. Accurate quantification of bacterial serine lipid, specifically lipid 654 [((S)-15-methyl-3-((13-methyltetradecanoyl)oxy)hexadecanoyl)glycyl-l-serine, (3S)-l-serine] isolated from Porphyromonas gingivalis, in biological samples requires the preparation of a stable isotope internal standard for sample supplementation and subsequent mass spectrometric analysis. This report describes the convergent synthesis of a deuterium-substituted serine dipeptide lipid, which is an isotopically labeled homologue that represents a dominant form of serine dipeptide lipid recovered in bacteria. Copyright © 2017 John Wiley & Sons, Ltd.

  11. Synthesis of surface nano-molecularly imprinted polymers for sensitive baicalin detection from biological samples.

    Science.gov (United States)

    Gu, Xiaoli; He, Hongliang; Wang, Chong-Zhi; Gao, Yankun; Zhang, Hongjuan; Hong, Junli; Du, Shuhu; Chen, Lina; Yuan, Chun-Su

    2015-01-01

    Surface molecularly imprinted polymers (MIP@SBA-15) imprinted on the surface of hybrid nanostructured organic/inorganic materials (SBA-15) were prepared for the selective extraction and detection of baicalin (BA) from biological samples. The surface morphologies and characteristics of the imprinted and non-imprinted polymers were characterized by Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermo-gravimetric analysis (TGA) and nitrogen adsorption-desorption isotherms. The results indicated that the polymers were successfully grafted on the surface of SBA-15 and possessed a highly ordered mesoporous structure. In binding tests, MIP@SBA-15 reached saturated adsorption within 80 min and exhibited significant specific recognition toward BA with large adsorption capacity. Meanwhile, the prepared MIP@SBA-15 was used as a selective sorbent for solid-phase extraction of BA from biological samples. Recoveries of BA from the liver and spleen ranged from 90.6% to 90.9% with RSD < 3.7%. All these results reveal that this method is simple, rapid and sensitive for effectively extracting and detecting trace BA in biological samples.

  12. Human biological sample biobanking to support tissue biomarkers in pharmaceutical research and development.

    Science.gov (United States)

    Womack, Christopher; Mager, S Rachel

    2014-11-01

    Advances in the understanding of molecular pathology and thereby the mechanisms that could be amenable to therapeutic manipulation are the reason that pharmaceutical research and development is focused increasingly on measurement of molecular biomarkers in human biological samples. Obtaining direct or indirect access to sufficient samples that are fit for research purposes can be a major challenge. A biobanking infrastructure has a significant role in the acquisition, storage and usage of human biological samples and here we review some key requirements for establishing a biobank. These include ensuring; that appropriate governance mechanisms are in place, that samples available are appropriate and fit for the intended research purposes that the infrastructure is sustainable in the future and that use of the biobank assets meets the strategic aims of the host organisation. Finally we present a case study--the STRATUM project which has recently completed and through a collaborative approach involving six industry and public partners drawing on a network of experts, examined biobank policies, public attitudes to biobanking, donor consent, sample and data standards, technical requirements for a register and biobanking financial models, albeit from a UK perspective. Copyright © 2014 Elsevier Inc. All rights reserved.

  13. Sampling designs matching species biology produce accurate and affordable abundance indices.

    Science.gov (United States)

    Harris, Grant; Farley, Sean; Russell, Gareth J; Butler, Matthew J; Selinger, Jeff

    2013-01-01

    Wildlife biologists often use grid-based designs to sample animals and generate abundance estimates. Although sampling in grids is theoretically sound, in application, the method can be logistically difficult and expensive when sampling elusive species inhabiting extensive areas. These factors make it challenging to sample animals and meet the statistical assumption of all individuals having an equal probability of capture. Violating this assumption biases results. Does an alternative exist? Perhaps by sampling only where resources attract animals (i.e., targeted sampling), it would provide accurate abundance estimates more efficiently and affordably. However, biases from this approach would also arise if individuals have an unequal probability of capture, especially if some failed to visit the sampling area. Since most biological programs are resource limited, and acquiring abundance data drives many conservation and management applications, it becomes imperative to identify economical and informative sampling designs. Therefore, we evaluated abundance estimates generated from grid and targeted sampling designs using simulations based on geographic positioning system (GPS) data from 42 Alaskan brown bears (Ursus arctos). Migratory salmon drew brown bears from the wider landscape, concentrating them at anadromous streams. This provided a scenario for testing the targeted approach. Grid and targeted sampling varied by trap amount, location (traps placed randomly, systematically or by expert opinion), and traps stationary or moved between capture sessions. We began by identifying when to sample, and if bears had equal probability of capture. We compared abundance estimates against seven criteria: bias, precision, accuracy, effort, plus encounter rates, and probabilities of capture and recapture. One grid (49 km(2) cells) and one targeted configuration provided the most accurate results. Both placed traps by expert opinion and moved traps between capture sessions

  14. Sampling designs matching species biology produce accurate and affordable abundance indices

    Directory of Open Access Journals (Sweden)

    Grant Harris

    2013-12-01

    Full Text Available Wildlife biologists often use grid-based designs to sample animals and generate abundance estimates. Although sampling in grids is theoretically sound, in application, the method can be logistically difficult and expensive when sampling elusive species inhabiting extensive areas. These factors make it challenging to sample animals and meet the statistical assumption of all individuals having an equal probability of capture. Violating this assumption biases results. Does an alternative exist? Perhaps by sampling only where resources attract animals (i.e., targeted sampling, it would provide accurate abundance estimates more efficiently and affordably. However, biases from this approach would also arise if individuals have an unequal probability of capture, especially if some failed to visit the sampling area. Since most biological programs are resource limited, and acquiring abundance data drives many conservation and management applications, it becomes imperative to identify economical and informative sampling designs. Therefore, we evaluated abundance estimates generated from grid and targeted sampling designs using simulations based on geographic positioning system (GPS data from 42 Alaskan brown bears (Ursus arctos. Migratory salmon drew brown bears from the wider landscape, concentrating them at anadromous streams. This provided a scenario for testing the targeted approach. Grid and targeted sampling varied by trap amount, location (traps placed randomly, systematically or by expert opinion, and traps stationary or moved between capture sessions. We began by identifying when to sample, and if bears had equal probability of capture. We compared abundance estimates against seven criteria: bias, precision, accuracy, effort, plus encounter rates, and probabilities of capture and recapture. One grid (49 km2 cells and one targeted configuration provided the most accurate results. Both placed traps by expert opinion and moved traps between capture

  15. Sampling designs matching species biology produce accurate and affordable abundance indices

    Science.gov (United States)

    Farley, Sean; Russell, Gareth J.; Butler, Matthew J.; Selinger, Jeff

    2013-01-01

    Wildlife biologists often use grid-based designs to sample animals and generate abundance estimates. Although sampling in grids is theoretically sound, in application, the method can be logistically difficult and expensive when sampling elusive species inhabiting extensive areas. These factors make it challenging to sample animals and meet the statistical assumption of all individuals having an equal probability of capture. Violating this assumption biases results. Does an alternative exist? Perhaps by sampling only where resources attract animals (i.e., targeted sampling), it would provide accurate abundance estimates more efficiently and affordably. However, biases from this approach would also arise if individuals have an unequal probability of capture, especially if some failed to visit the sampling area. Since most biological programs are resource limited, and acquiring abundance data drives many conservation and management applications, it becomes imperative to identify economical and informative sampling designs. Therefore, we evaluated abundance estimates generated from grid and targeted sampling designs using simulations based on geographic positioning system (GPS) data from 42 Alaskan brown bears (Ursus arctos). Migratory salmon drew brown bears from the wider landscape, concentrating them at anadromous streams. This provided a scenario for testing the targeted approach. Grid and targeted sampling varied by trap amount, location (traps placed randomly, systematically or by expert opinion), and traps stationary or moved between capture sessions. We began by identifying when to sample, and if bears had equal probability of capture. We compared abundance estimates against seven criteria: bias, precision, accuracy, effort, plus encounter rates, and probabilities of capture and recapture. One grid (49 km2 cells) and one targeted configuration provided the most accurate results. Both placed traps by expert opinion and moved traps between capture sessions, which

  16. Purification and concentration of lead samples in biological monitoring of occupational exposures

    Directory of Open Access Journals (Sweden)

    A Rahimi-Froushani

    2006-04-01

    Full Text Available Background and Aims:Lead is an important environmental constituent widely used in industrialprocesses for production of synthetic materials and therefore can be released in the environmentcausing public exposure especially around the industrial residence area. For evaluation of humanexposure to trace toxic metal of Pb (II, environmental and biological monitoring are essentialprocesses, in which, preparation of such samples is one of the most time-consuming and errorproneaspects prior to analysis. The use of solid-phase extraction (SPE has grown and is a fertiletechnique of sample preparation as it provides better results than those produced by liquid-liquidextraction (LLE. The aim of this study was to investigate factors influencing sample pretreatmentfor trace analysis of lead in biological samples for evaluation of occupational exposure.Method :To evaluate factors influencing quantitative analysis scheme of lead, solid phaseextraction using mini columns filled with XAD-4 resin was optimized with regard to sample pH,ligand concentration, loading flow rate, elution solvent, sample volume (up to 500 ml, elutionvolume, amount of resins, and sample matrix interferences.Results :Lead was retained on solid sorbent and eluted followed by simple determination ofanalytes by using flame atomic absorption spectrometery. Obtained recoveries of the metal ionwere more than 92%. The amount of the analyte detected after simultaneous pre-concentrationwas basically in agreement with the added amounts. The optimized procedure was also validatedwith three different pools of spiked urine samples and showed a good reproducibility over sixconsecutive days as well as six within-day experiments. The developed method promised to beapplicable for evaluation of other metal ions present in different environmental and occupationalsamples as suitable results were obtained for relative standard deviation (less than 10%.Conclusion:This optimized method can be considered to be

  17. Preconcentration and determination of heavy metals in water, sediment and biological samples

    Directory of Open Access Journals (Sweden)

    Shirkhanloo Hamid

    2011-01-01

    Full Text Available In this study, a simple, sensitive and accurate column preconcentration method was developed for the determination of Cd, Cu and Pb ions in river water, urine and sediment samples by flame atomic absorption spectrometry. The procedure is based on the retention of the analytes on a mixed cellulose ester membrane (MCEM column from buffered sample solutions and then their elution from the column with nitric acid. Several parameters, such as pH of the sample solution, volume of the sample and eluent and flow rates of the sample were evaluated. The effects of diverse ions on the preconcentration were also investigated. The recoveries were >95 %. The developed method was applied to the determination of trace metal ions in river water, urine and sediment samples, with satisfactory results. The 3δ detection limits for Cu, Pb and Cd were found to be 2, 3 and 0.2 μg dm−3, respectively. The presented procedure was successfully applied for determination of the copper, lead and cadmium contents in real samples, i.e., river water and biological samples.

  18. Simultaneous AMS determination of {sup 14}C content and total carbon mass in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Zoppi, U., E-mail: uzoppi@acciumbio.co [Accium BioSciences, 550 17th Avenue, Suite 550, Seattle, WA 98122 (United States); Arjomand, A. [Accium BioSciences, 550 17th Avenue, Suite 550, Seattle, WA 98122 (United States)

    2010-04-15

    Accelerator Mass Spectrometry (AMS) is now recognized as one of the most powerful techniques available for conducting ultrasensitive clinical studies. However, since for biological applications the relevant quantity is the total {sup 14}C activity (i.e. dpm/mL sample), AMS {sup 14}C measurements must be combined with total carbon concentrations measured on a separate instrument using a different sample aliquot. This procedure is inherently a source of large inaccuracies, especially in non-homogeneous samples such as urine and fecal blends. To overcome this limitation we developed a new measurement technique whereby a small amount of {sup 13}C-enriched carbon carrier is added to each sample. Accurate measurement of the {sup 13}C/{sup 12}C and {sup 14}C/{sup 13}C ratios of the mix can be used to simultaneously calculate total carbon mass and {sup 14}C concentration of the original sample. In this paper we present our first test runs including a detailed error analysis demonstrating that sample mass and {sup 14}C concentration of the original sample can be determined with a precision and accuracy of better than 3%, thus significantly reducing the final uncertainty due to sample in-homogeneities.

  19. Sampling and Analysis Instruction for the Demolition of the Masonry Block for the 108-F Biological Laboratory

    International Nuclear Information System (INIS)

    Byrnes, M. E.

    1999-01-01

    This sampling and analysis instruction (SAI) has been prepared to clearly define the sampling and analysis activities to be performed in support of the demolition and disposition (or disposal) of the 108-F Biological Laboratory masonry block walls

  20. Evaluation of a gas chromatography method for azelaic acid determination in selected biological samples.

    Science.gov (United States)

    Garelnabi, Mahdi; Litvinov, Dmitry; Parthasarathy, Sampath

    2010-09-01

    Azelaic acid (AzA) is the best known dicarboxilic acid to have pharmaceutical benefits and clinical applications and also to be associated with some diseases pathophysiology. We extracted and methylesterified AzA and determined its concentration in human plasma obtained from healthy individuals and also in mice fed AzA containing diet for three months. AzA was detected in Gas Chromatography (GC) and confirmed by Liquid chromatography mass spectrometry (LCMS), and gas chromatography mass spectrometry (GCMC). Our results have shown that AzA can be determined efficiently in selected biological samples by GC method with 1nM limit of detection (LoD) and the limit of quantification (LoQ); was established at 50nM. Analytical Sensitivity as assayed by hexane demonstrated an analytical sensitivity at 0.050nM. The method has demonstrated 8-10% CV batch repeatability across the sample types and 13-18.9% CV for the Within-Lab Precision analysis. The method has shown that AzA can efficiently be recovered from various sample preparation including liver tissue homogenate (95%) and human plasma (97%). Because of its simplicity and lower limit of quantification, the present method provides a useful tool for determining AzA in various biological sample preparations.

  1. Controlled power delivery for super-resolution imaging of biological samples using digital micromirror device

    Science.gov (United States)

    Valiya Peedikakkal, Liyana; Cadby, Ashley

    2017-02-01

    Localization based super resolution images of a biological sample is generally achieved by using high power laser illumination with long exposure time which unfortunately increases photo-toxicity of a sample, making super resolution microscopy, in general, incompatible with live cell imaging. Furthermore, the limitation of photobleaching reduces the ability to acquire time lapse images of live biological cells using fluorescence microscopy. Digital Light Processing (DLP) technology can deliver light at grey scale levels by flickering digital micromirrors at around 290 Hz enabling highly controlled power delivery to samples. In this work, Digital Micromirror Device (DMD) is implemented in an inverse Schiefspiegler telescope setup to control the power and pattern of illumination for super resolution microscopy. We can achieve spatial and temporal patterning of illumination by controlling the DMD pixel by pixel. The DMD allows us to control the power and spatial extent of the laser illumination. We have used this to show that we can reduce the power delivered to the sample to allow for longer time imaging in one area while achieving sub-diffraction STORM imaging in another using higher power densities.

  2. Biological rhythms, metabolic syndrome and current depressive episode in a community sample.

    Science.gov (United States)

    Moreira, Fernanda Pedrotti; Jansen, Karen; Mondin, Thaíse Campos; Cardoso, Taiane de Azevedo; Magalhães, Pedro Vieira da Silva; Kapczinski, Flavio; Frey, Benicio N; Oses, Jean Pierre; Souza, Luciano Dias de Mattos; da Silva, Ricardo Azevedo; Wiener, Carolina David

    2016-10-01

    The purpose of this study was to assess the disruption in biological rhythms and metabolic syndrome (MetS) in individuals with depressive episode. This was a cross-sectional, population-based study with a representative sample of 905 young adults. Current depressive episode were confirmed by a psychologist using the Mini International Neuropsychiatric Interview (MINI)-Plus. Self-reported biological rhythms were assessed using the Biological Rhythms Interview of Assessment in Neuropsychiatry (BRIAN). MetS was defined using modified NCEP/ATPIII criteria. Significant main effects of current depressive episode (pbiological rhythm scores (p=0.002, η(2)=0.011) as well as sleep (p=0.001, η(2)=0.016) and social domains (pbiological rhythms are associated with key components of the MetS in community adults with MDD. The understanding of the complex interactions between biological rhythms, MetS and depression are important in the development of preventive and therapeutic strategies. Copyright © 2016 Elsevier Ltd. All rights reserved.

  3. Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

    International Nuclear Information System (INIS)

    Chandra, Subhash

    2008-01-01

    Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2 + ) revealed local secondary ion signal enhancements correlated with the water image signals of 19 (H 3 O) + . A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells

  4. Challenges of biological sample preparation for SIMS imaging of elements and molecules at subcellular resolution

    Science.gov (United States)

    Chandra, Subhash

    2008-12-01

    Secondary ion mass spectrometry (SIMS) based imaging techniques capable of subcellular resolution characterization of elements and molecules are becoming valuable tools in many areas of biology and medicine. Due to high vacuum requirements of SIMS, the live cells cannot be analyzed directly in the instrument. The sample preparation, therefore, plays a critical role in preserving the native chemical composition for SIMS analysis. This work focuses on the evaluation of frozen-hydrated and frozen freeze-dried sample preparations for SIMS studies of cultured cells with a CAMECA IMS-3f dynamic SIMS ion microscope instrument capable of producing SIMS images with a spatial resolution of 500 nm. The sandwich freeze-fracture method was used for fracturing the cells. The complimentary fracture planes in the plasma membrane were characterized by field-emission secondary electron microscopy (FESEM) in the frozen-hydrated state. The cells fractured at the dorsal surface were used for SIMS analysis. The frozen-hydrated SIMS analysis of individual cells under dynamic primary ion beam (O 2+) revealed local secondary ion signal enhancements correlated with the water image signals of 19(H 3O) +. A preferential removal of water from the frozen cell matrix in the Z-axis was also observed. These complications render the frozen-hydrated sample type less desirable for subcellular dynamic SIMS studies. The freeze-drying of frozen-hydrated cells, either inside the instrument or externally in a freeze-drier, allowed SIMS imaging of subcellular chemical composition. Morphological evaluations of fractured freeze-dried cells with SEM and confocal laser scanning microscopy (CLSM) revealed well-preserved mitochondria, Golgi apparatus, and stress fibers. SIMS analysis of fractured freeze-dried cells revealed well-preserved chemical composition of even the most highly diffusible ions like K + and Na + in physiologically relevant concentrations. The high K-low Na signature in individual cells

  5. MALDI-MS drug analysis in biological samples: opportunities and challenges.

    Science.gov (United States)

    Steuer, Andrea E; Poetzsch, Michael; Kraemer, Thomas

    2016-09-01

    Drug analysis represents a large field in different disciplines. Plasma is commonly considered to be the biosample of choice for that purpose. However, concentrations often do not represent the levels present within deeper compartments and therefore cannot sufficiently explain efficacy or toxicology of drugs. MALDI-MS in drug analysis is of great interest for high-throughput quantification and particularly spatially resolved tissue imaging. The current perspective article will deal with challenges and opportunities of MALDI-MS drug analysis in different biological samples. A particular focus will be on hair samples. Recent applications were included, reviewed for their instrumental setup and sample preparation and pros and cons as well as future perspectives are critically discussed.

  6. Crystallization of biological macromolecules from flash frozen samples on the Russian Space Station Mir.

    Science.gov (United States)

    Koszelak, S; Leja, C; McPherson, A

    1996-11-20

    One hundred eighty-three flash frozen, liquid-liquid diffusion and batch method protein and virus crystallization samples were launched aboard the Space Shuttle Discovery on June 27 (STS-71) and transferred to the Russian Space Station Mir on July 1, 1995. They were returned to earth November 20, 1995 (STS-74). Subsequent examination showed that of the 19 types of proteins and viruses investigated, 17 were crystallized during the period on Mir. The experiment demonstrates the utility of this very simple and inexpensive approach for the crystallization of biological macromolecules in space over extended time periods. The distribution of crystals among the three types of containers used indicated small samples yielded results equal or better than larger samples and that long diffusion path lengths were clearly better. Distribution of crystals within the container tubes showed a striking gradient of quality and size that indicated long, narrow tubes yield superior crystals, as predicted from other work based on crystallization in capillaries.

  7. A direct solid sampling analysis method for the detection of silver nanoparticles in biological matrices.

    Science.gov (United States)

    Feichtmeier, Nadine S; Ruchter, Nadine; Zimmermann, Sonja; Sures, Bernd; Leopold, Kerstin

    2016-01-01

    Engineered silver nanoparticles (AgNPs) are implemented in food contact materials due to their powerful antimicrobial properties and so may enter the human food chain. Hence, it is desirable to develop easy, sensitive and fast analytical screening methods for the determination of AgNPs in complex biological matrices. This study describes such a method using solid sampling high-resolution continuum source graphite furnace atomic absorption spectrometry (GFAAS). A recently reported novel evaluation strategy uses the atomization delay of the respective GFAAS signal as significant indicator for AgNPs and thereby allows discrimination of AgNPs from ionic silver (Ag(+)) in the samples without elaborate sample pre-treatment. This approach was further developed and applied to a variety of biological samples. Its suitability was approved by investigation of eight different food samples (parsley, apple, pepper, cheese, onion, pasta, maize meal and wheat flour) spiked with ionic silver or AgNPs. Furthermore, the migration of AgNPs from silver-impregnated polypropylene food storage boxes to fresh pepper was observed and a mussel sample obtained from a laboratory exposure study with silver was investigated. The differences in the atomization delays (Δt(ad)) between silver ions and 20-nm AgNPs vary in a range from -2.01 ± 1.38 s for maize meal to +2.06 ± 1.08 s for mussel tissue. However, the differences were significant in all investigated matrices and so indicative of the presence/absence of AgNPs. Moreover, investigation of model matrices (cellulose, gelatine and water) gives the first indication of matrix-dependent trends. Reproducibility and homogeneity tests confirm the applicability of the method.

  8. Spectrochemical analysis of powdered biological samples using transversely excited atmospheric carbon dioxide laser plasma excitation

    Science.gov (United States)

    Zivkovic, Sanja; Momcilovic, Milos; Staicu, Angela; Mutic, Jelena; Trtica, Milan; Savovic, Jelena

    2017-02-01

    The aim of this study was to develop a simple laser induced breakdown spectroscopy (LIBS) method for quantitative elemental analysis of powdered biological materials based on laboratory prepared calibration samples. The analysis was done using ungated single pulse LIBS in ambient air at atmospheric pressure. Transversely-Excited Atmospheric pressure (TEA) CO2 laser was used as an energy source for plasma generation on samples. The material used for the analysis was a blue-green alga Spirulina, widely used in food and pharmaceutical industries and also in a few biotechnological applications. To demonstrate the analytical potential of this particular LIBS system the obtained spectra were compared to the spectra obtained using a commercial LIBS system based on pulsed Nd:YAG laser. A single sample of known concentration was used to estimate detection limits for Ba, Ca, Fe, Mg, Mn, Si and Sr and compare detection power of these two LIBS systems. TEA CO2 laser based LIBS was also applied for quantitative analysis of the elements in powder Spirulina samples. Analytical curves for Ba, Fe, Mg, Mn and Sr were constructed using laboratory produced matrix-matched calibration samples. Inductively coupled plasma optical emission spectroscopy (ICP-OES) was used as the reference technique for elemental quantification, and reasonably well agreement between ICP and LIBS data was obtained. Results confirm that, in respect to its sensitivity and precision, TEA CO2 laser based LIBS can be successfully applied for quantitative analysis of macro and micro-elements in algal samples. The fact that nearly all classes of materials can be prepared as powders implies that the proposed method could be easily extended to a quantitative analysis of different kinds of materials, organic, biological or inorganic.

  9. Monitoring prion protein expression in complex biological samples by SERS for diagnostic applications

    International Nuclear Information System (INIS)

    Manno, D; Filippo, E; Fiore, R; Serra, A; Urso, E; Rizzello, A; Maffia, M

    2010-01-01

    Surface-enhanced Raman spectroscopy (SERS) allows a new insight into the analysis of cell physiology. In this work, the difficulty of producing suitable substrates that, besides permitting the amplification of the Raman signal, do not interact with the biological material causing alteration, has been overcome by a combined method of hydrothermal green synthesis and thermal annealing. The SERS analysis of the cell membrane has been performed with special attention to the cellular prion protein PrP C . In addition, SERS has also been used to reveal the prion protein-Cu(II) interaction in four different cell models (B104, SH-SY5Y, GN11, HeLa), expressing PrP C at different levels. A significant implication of the current work consists of the intriguing possibility of revealing and quantifying prion protein expression in complex biological samples by a cheap SERS-based method, replacing the expensive and time-consuming immuno-assay systems commonly employed.

  10. Development of an improved immunoassay for detection of sorLA in cells and biological samples

    DEFF Research Database (Denmark)

    Andersen, Olav Michael; Thakurta, Ishita Guha; West, Mark J.

    Background: SorLA (Sorting - related receptor with A- type repeats) is a 250 kDa type I transmembrane protein, belonging to the VPS10P (vacuolar protein sorting 10 protein) family of neuronal receptors. It is implicated in the development of AD (Alzheimer's Disease), atherosclerosis, diabetic...... retinopathy, and acute leukemia. Despite the overwhelming evidence regarding the role of sorLA in various diseases, there has been a lack of technologies which can precisely quantitate the levels of sorLA in various complex biological matrices. The methods are either qualitative like immunohistochemistry......, or traditional sandwich ELISA assays which are time consuming and less sensitive. Hence, the purpose of the present study is to develop a new assay called AlphaLISA which is fast and very sensitive, to measure sorLA in extremely small volumes of cells and biological samples. Methods: The Alpha...

  11. Development of an improved immunoassay for detection of sorLA in cells and biological samples

    DEFF Research Database (Denmark)

    Andersen, Olav Michael; Thakurta, Ishita Guha; West, Mark J.

    retinopathy, and acute leukemia. Despite the overwhelming evidence regarding the role of sorLA in various diseases, there has been a lack of technologies which can precisely quantitate the levels of sorLA in various complex biological matrices. The methods are either qualitative like immunohistochemistry......, or traditional sandwich ELISA assays which are time consuming and less sensitive. Hence, the purpose of the present study is to develop a new assay called AlphaLISA which is fast and very sensitive, to measure sorLA in extremely small volumes of cells and biological samples. Methods: The Alpha...... bead releases singlet oxygen which triggers a series of chemical reactions in the acceptor beads causing a sharp peak of light emission at 615 nm. A series of experiments were designed to optimize the assay by conjugation of the beads to various anti-sorLA antibodies, cross titrations of the antibodies...

  12. Method and apparatus for imaging substances in biological samples by nuclear magnetic resonance

    International Nuclear Information System (INIS)

    Shaw, D.

    1984-01-01

    A method of determining the distribution of non-proton nuclei having a magnetic moment in a biological sample is described. It comprises subjecting the sample to a magnetic field, irradiating the sample with RF radiation at a proton magnetic resonance frequency and deriving a first NMR signal, indicative of electromagnetic absorption of the sample at the proton magnetic resonance frequency. A second such NMR signal at the proton resonance frequency is then derived from the sample in the presence of RF radiation at the nuclear magnetic resonance frequency of the non-proton nuclei so as to decouple protons in the sample from the non-proton nuclei. By applying an imaging technique, an image indicative of the spatial variation of the difference between the first and second signals can be produced. Imaging may be performed on the difference between the two NMR signals, or on each NMR signal followed by subtraction of the images. The method can be used to trace how a 13 C-labelled material introduced into a patient, and its breakdown products, become distributed. (author)

  13. Analysis of biological slurry samples by total x-ray fluorescence after in situ microwave digestion

    International Nuclear Information System (INIS)

    Lue-Meru, M.P.; Capote, T.; Greaves, E.

    2000-01-01

    Biological slurry samples were analyzed by total reflection x-ray fluorescence (TXRF) after an in situ microwave digestion procedure on the quartz reflector. This method lead to the removal of the matrix by the digestion and permits the enrichment of the analites by using sample amounts higher than those normally used in TXRF for the thin layer requirement since the organic matrix is removed. In consequence, the pre-concentration of sample is performed and the detection capability is increased by a quasi direct method. The samples analyzed were the international IAEA blood standard, the SRM bovine liver 1577-a standard and fresh onion tissues. Slurries were prepared in three ways: a.- weighing a sample amount on the reflector and adding suprapure nitric acid and internal standard followed by microwave digestion, b.-weighing a sample amount and water with an appropriate concentration of the internal standard in an Eppendorf vial, taking then an aliquot to the quartz reflector for microwave digestion with suprapure nitric acid, c.- weighing a sample amount of fresh tissue, homogenising with high speed homegenator to obtain a slurry sample which can be diluted in an ependorf vial with water an the internal standard. Then an aliquot is taken to the reflector for microwave digestion with suprapure nitric acid. Further details of sample preparation procedures will be discussed during presentation. The analysis was carried out in a Canberra spectrometer using the Kalpha lines of the Ag and Mo tubes. The elements Ca, K, Fe, Cu, Zn, Se, Mn, Rb, Br, Sr were determined. The effect of the preparation procedure was evaluated by the accuracy and precision of the results for each element and the percent of recovery. (author)

  14. Highly sensitive quantification of key regulatory oxysterols in biological samples by LC-ESI-MS/MS.

    Science.gov (United States)

    Honda, Akira; Yamashita, Kouwa; Hara, Takashi; Ikegami, Tadashi; Miyazaki, Teruo; Shirai, Mutsumi; Xu, Guorong; Numazawa, Mitsuteru; Matsuzaki, Yasushi

    2009-02-01

    We describe a highly sensitive and specific method for the quantification of key regulatory oxysterols in biological samples. This method is based upon a stable isotope dilution technique by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After alkaline hydrolysis of human serum (5 microl) or rat liver microsomes (1 mg protein), oxysterols were extracted, derivatized into picolinyl esters, and analyzed by LC-MS/MS using the electrospray ionization mode. The detection limits of the picolinyl esters of 4beta-hydroxycholesterol, 7alpha-hydroxycholesterol, 22R-hydroxycholesterol, 24S-hydroxycholesterol, 25-hydroxycholesterol, 27-hydroxycholesterol, and 24S,25-epoxycholesterol were 2-10 fg (5-25 amol) on-column (signal-to-noise ratio = 3). Reproducibilities and recoveries of these oxysterols were validated according to one-way layout and polynomial equation, respectively. The variances between sample preparations and between measurements by this method were calculated to be 1.8% to 12.7% and 2.9% to 11.9%, respectively. The recovery experiments were performed using rat liver microsomes spiked with 0.05 ng to 12 ng of oxysterols, and recoveries of the oxysterols ranged from 86.7% to 107.3%, with a mean recovery of 100.6%. This method provides reproducible and reliable results for the quantification of oxysterols in small amounts of biological samples.

  15. Bioanalytical methods for the determination of cocaine and metabolites in human biological samples.

    Science.gov (United States)

    Barroso, M; Gallardo, E; Queiroz, J A

    2009-08-01

    Determination of cocaine and its metabolites in biological specimens is of great importance, not only in clinical and forensic toxicology, but also in workplace drug testing. These compounds are normally screened for using sensitive immunological methods. However, screening methods are unspecific and, therefore, the posterior confirmation of presumably positive samples by a specific technique is mandatory. Although GC-MS-based techniques are still the most commonly used for confirmation purposes of cocaine and its metabolites in biological specimens, the advent of LC-MS and LC-MS/MS has enabled the detection of even lower amounts of these drugs, which assumes particular importance when sample volume available is small, as frequently occurs with oral fluid. This paper will review recently-published papers that describe procedures for detection of cocaine and metabolites, not only in the most commonly used specimens, such as blood and urine, but also in other 'alternative' matrices (e.g., oral fluid and hair) with a special focus on sample preparation and chromatographic analysis.

  16. Magnetic induction spectroscopy: non-contact measurement of the electrical conductivity spectra of biological samples

    International Nuclear Information System (INIS)

    Barai, A; Watson, S; Patz, R; Griffiths, H

    2012-01-01

    Measurement of the electrical conductivity of biological tissues as a function of frequency, often termed ‘bioelectrical impedance spectroscopy (BIS)’, provides valuable information on tissue structure and composition. In implementing BIS though, there can be significant practical difficulties arising from the electrode–sample interface which have likely limited its deployment in industrial applications. In magnetic induction spectroscopy (MIS) these difficulties are eliminated through the use of fully non-contacting inductive coupling between the sensors and sample. However, inductive coupling introduces its own set of technical difficulties, primarily related to the small magnitudes of the induced currents and their proportionality with frequency. This paper describes the design of a practical MIS system incorporating new, highly-phase-stable electronics and compares its performance with that of electrode-based BIS in measurements on biological samples including yeast suspensions in saline (concentration 50–400 g l −1 ) and solid samples of potato, cucumber, tomato, banana and porcine liver. The shapes of the MIS spectra were in good agreement with those for electrode-based BIS, with a residual maximum discrepancy of 28%. The measurement precision of the MIS was 0.05 S m −1 at 200 kHz, improving to 0.01 S m −1 at a frequency of 20 MHz, for a sample volume of 80 ml. The data-acquisition time for each MIS measurement was 52 s. Given the value of spectroscopic conductivity information and the many advantages of obtaining these data in a non-contacting manner, even through electrically-insulating packaging materials if necessary, it is concluded that MIS is a technique with considerable potential for monitoring bio-industrial processes and product quality. (paper)

  17. Carbon and nitrogen isotope analysis for amino acids from biological sample

    Energy Technology Data Exchange (ETDEWEB)

    Minagawa, Masao; Egawa, Saho; Kabaya, Yuko; Karasawa-Tsuru, Kyoko (Mitsubishi Kasei Inst. of Life Sciences, Machida, Tokyo (Japan))

    1992-02-01

    Evaluation was made for carbon and nitrogen stable isotope analyses of amino acids which were hydrolyzed from biological samples. Alteration of isotopic compositions during chemical preparations was studied in incorporation with organic solvent, acid hydrolysis, and ion-exchange chromatography. Based on such assessment, analyses of isotope compositions of single amino acids were made for collagen and plant protein. The carbon isotope composition of soybean showed consistent pattern with algal amino acids. Similarity was also found in the intermolecular relationship of {delta}{sup 13}C and {delta}{sup 15}N between collagen and soybean protein. (author).

  18. DESIGN OF A SIMPLE SLOW COOLING DEVICE FOR CRYOPRESERVATION OF SMALL BIOLOGICAL SAMPLES.

    Science.gov (United States)

    de Paz, Leonardo Juan; Robert, Maria Celeste; Graf, Daniel Adolfo; Guibert, Edgardo Elvio; Rodriguez, Joaquin Valentin

    2015-01-01

    Slow cooling is a cryopreservation methodology where samples are cooled to its storage temperature at controlled cooling rates. Design, construction and evaluation of a simple and low cost device for slow cooling of small biological samples. The device was constructed based on Pye's freezer idea. A Dewar flask filled with liquid nitrogen was used as heat sink and a methanol bath containing the sample was cooled at constant rates using copper bars as heat conductor. Sample temperature may be lowered at controlled cooling rate (ranging from 0.4°C/min to 6.0°C/min) down to ~-60°C, where it could be conserved at lower temperatures. An example involving the cryopreservation of Neuro-2A cell line showed a marked influence of cooling rate over post preservation cell viability with optimal values between 2.6 and 4.6°C/min. The cooling device proved to be a valuable alternative to more expensive systems allowing the assessment of different cooling rates to evaluate the optimal condition for cryopreservation of such samples.

  19. Sample sizing of biological materials analyzed by energy dispersion X-ray fluorescence

    International Nuclear Information System (INIS)

    Paiva, Jose D.S.; Franca, Elvis J.; Magalhaes, Marcelo R.L.; Almeida, Marcio E.S.; Hazin, Clovis A.

    2013-01-01

    Analytical portions used in chemical analyses are usually less than 1g. Errors resulting from the sampling are barely evaluated, since this type of study is a time-consuming procedure, with high costs for the chemical analysis of large number of samples. The energy dispersion X-ray fluorescence - EDXRF is a non-destructive and fast analytical technique with the possibility of determining several chemical elements. Therefore, the aim of this study was to provide information on the minimum analytical portion for quantification of chemical elements in biological matrices using EDXRF. Three species were sampled in mangroves from the Pernambuco, Brazil. Tree leaves were washed with distilled water, oven-dried at 60 deg C and milled until 0.5 mm particle size. Ten test-portions of approximately 500 mg for each species were transferred to vials sealed with polypropylene film. The quality of the analytical procedure was evaluated from the reference materials IAEA V10 Hay Powder, SRM 2976 Apple Leaves. After energy calibration, all samples were analyzed under vacuum for 100 seconds for each group of chemical elements. The voltage used was 15 kV and 50 kV for chemical elements of atomic number lower than 22 and the others, respectively. For the best analytical conditions, EDXRF was capable of estimating the sample size uncertainty for further determination of chemical elements in leaves. (author)

  20. Sample sizing of biological materials analyzed by energy dispersion X-ray fluorescence

    Energy Technology Data Exchange (ETDEWEB)

    Paiva, Jose D.S.; Franca, Elvis J.; Magalhaes, Marcelo R.L.; Almeida, Marcio E.S.; Hazin, Clovis A., E-mail: dan-paiva@hotmail.com, E-mail: ejfranca@cnen.gov.br, E-mail: marcelo_rlm@hotmail.com, E-mail: maensoal@yahoo.com.br, E-mail: chazin@cnen.gov.b [Centro Regional de Ciencias Nucleares do Nordeste (CRCN-NE/CNEN-PE), Recife, PE (Brazil)

    2013-07-01

    Analytical portions used in chemical analyses are usually less than 1g. Errors resulting from the sampling are barely evaluated, since this type of study is a time-consuming procedure, with high costs for the chemical analysis of large number of samples. The energy dispersion X-ray fluorescence - EDXRF is a non-destructive and fast analytical technique with the possibility of determining several chemical elements. Therefore, the aim of this study was to provide information on the minimum analytical portion for quantification of chemical elements in biological matrices using EDXRF. Three species were sampled in mangroves from the Pernambuco, Brazil. Tree leaves were washed with distilled water, oven-dried at 60 deg C and milled until 0.5 mm particle size. Ten test-portions of approximately 500 mg for each species were transferred to vials sealed with polypropylene film. The quality of the analytical procedure was evaluated from the reference materials IAEA V10 Hay Powder, SRM 2976 Apple Leaves. After energy calibration, all samples were analyzed under vacuum for 100 seconds for each group of chemical elements. The voltage used was 15 kV and 50 kV for chemical elements of atomic number lower than 22 and the others, respectively. For the best analytical conditions, EDXRF was capable of estimating the sample size uncertainty for further determination of chemical elements in leaves. (author)

  1. Development and application of a micro-digestion device for biological samples

    International Nuclear Information System (INIS)

    Bohlen, A. von; Klockenkaemper, R.; Messerschmidt, J.; Alt, F.

    2000-01-01

    The analytical characterization of small amounts of a sample is of increasing importance for various research projects in biology, biochemistry and medicine. Reliable determinations of minor and trace elements in microsamples can be performed by total reflection x-ray fluorescence analysis (TXRF). This microanalytical method is suitable for direct multielement analyses of a tiny amount of a liquid or solid sample. Instead of a direct analysis, however, a complete digestion or mineralisation of the sample material prior to analysis can be recommendable. It can be advantageous for a favorable presentation, for a preconcentration and/or homogenization of the material and particularly for an accurate quantification. Unfortunately, commercially available digestion devices are optimized for amounts of 50 to 400 mg of a sample. For smaller amounts, a microdigestion device was constructed and adapted to an equipment of high pressure ashing, which is commercially available. Digestions of very different microsamples between some μg and some mg were carried out, followed by quantitative determinations of a lot of elements. Besides, different Standard Reference Materials (SRM) were analyzed. The homogeneity of these materials could be investigated by comparing the results found for microsamples with those obtained for samples of 200 mg, the latter after digestion in a conventional device. (author)

  2. Testosterone and progesterone concentrations in blow samples are biologically relevant in belugas (Delphinapterus leucas).

    Science.gov (United States)

    Richard, Justin T; Robeck, Todd R; Osborn, Steven D; Naples, Lisa; McDermott, Alexa; LaForge, Robert; Romano, Tracy A; Sartini, Becky L

    2017-05-15

    Steroid hormone analysis in blow (respiratory vapor) may provide a minimally invasive way to assess the reproductive status of wild cetaceans. Biological validation of the method is needed to allow for the interpretation of hormone measurements in blow samples. Utilizing samples collected from trained belugas (Delphinapterus leucas, n=20), enzyme immunoassays for testosterone and progesterone were validated for use with beluga blow samples. Testosterone concentrations in 40 matched blood and blow samples collected from 4 male belugas demonstrated a positive correlation (R 2 =0.52, pTestosterone concentrations (mean±SD) in blow samples collected from adult males (119.3±14.2pg/ml) were higher (ptestosterone concentrations in blow demonstrated a seasonal pattern of secretion, with peak secretion occurring during the breeding season (February-April, 136.95±33.8pg/ml). Progesterone concentrations in blow varied by reproductive status; pregnant females (410.6±87.8pg/ml) and females in the luteal phase of the estrous cycle (339.5±51.0pg/ml) had higher (ptestosterone or progesterone in belugas. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. Availability of MudPIT data for classification of biological samples.

    Science.gov (United States)

    Silvestre, Dario Di; Zoppis, Italo; Brambilla, Francesca; Bellettato, Valeria; Mauri, Giancarlo; Mauri, Pierluigi

    2013-01-14

    Mass spectrometry is an important analytical tool for clinical proteomics. Primarily employed for biomarker discovery, it is increasingly used for developing methods which may help to provide unambiguous diagnosis of biological samples. In this context, we investigated the classification of phenotypes by applying support vector machine (SVM) on experimental data obtained by MudPIT approach. In particular, we compared the performance capabilities of SVM by using two independent collection of complex samples and different data-types, such as mass spectra (m/z), peptides and proteins. Globally, protein and peptide data allowed a better discriminant informative content than experimental mass spectra (overall accuracy higher than 87% in both collection 1 and 2). These results indicate that sequencing of peptides and proteins reduces the experimental noise affecting the raw mass spectra, and allows the extraction of more informative features available for the effective classification of samples. In addition, proteins and peptides features selected by SVM matched for 80% with the differentially expressed proteins identified by the MAProMa software. These findings confirm the availability of the most label-free quantitative methods based on processing of spectral count and SEQUEST-based SCORE values. On the other hand, it stresses the usefulness of MudPIT data for a correct grouping of sample phenotypes, by applying both supervised and unsupervised learning algorithms. This capacity permit the evaluation of actual samples and it is a good starting point to translate proteomic methodology to clinical application.

  4. An introduction to sample preparation and imaging by cryo-electron microscopy for structural biology

    Science.gov (United States)

    Thompson, Rebecca F.; Walker, Matt; Siebert, C. Alistair; Muench, Stephen P.; Ranson, Neil A.

    2016-01-01

    Transmission electron microscopy (EM) is a versatile technique that can be used to image biological specimens ranging from intact eukaryotic cells to individual proteins >150 kDa. There are several strategies for preparing samples for imaging by EM, including negative staining and cryogenic freezing. In the last few years, cryo-EM has undergone a ‘resolution revolution’, owing to both advances in imaging hardware, image processing software, and improvements in sample preparation, leading to growing number of researchers using cryo-EM as a research tool. However, cryo-EM is still a rapidly growing field, with unique challenges. Here, we summarise considerations for imaging of a range of specimens from macromolecular complexes to cells using EM. PMID:26931652

  5. Towards a new method for the quantification of metabolites in the biological sample

    International Nuclear Information System (INIS)

    Neugnot, B.

    2005-03-01

    The quantification of metabolites is a key step in drug development. The aim of this Ph.D. work was to study the feasibility of a new method for this quantification, in the biological sample, without the drawbacks (cost, time, ethics) of the classical quantification methods based on metabolites synthesis or administration to man of the radiolabelled drug. Our strategy consists in determining the response factor, in mass spectrometry, of the metabolites. This approach is based on tritium labelling of the metabolites, ex vivo, by isotopic exchange. The labelling step was studied with deuterium. Metabolites of a model drug, recovered from in vitro or urinary samples, were labelled by three ways (Crab tree's catalyst ID2, deuterated trifluoroacetic acid or rhodium chloride ID20). Then, the transposition to tritium labelling was studied and the first results are very promising for the ultimate validation of the method. (author)

  6. Analytical Methodologies for the Determination of Endocrine Disrupting Compounds in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    Zoraida Sosa-Ferrera

    2013-01-01

    Full Text Available Endocrine-disruptor compounds (EDCs can mimic natural hormones and produce adverse effects in the endocrine functions by interacting with estrogen receptors. EDCs include both natural and synthetic chemicals, such as hormones, personal care products, surfactants, and flame retardants, among others. EDCs are characterised by their ubiquitous presence at trace-level concentrations and their wide diversity. Since the discovery of the adverse effects of these pollutants on wildlife and human health, analytical methods have been developed for their qualitative and quantitative determination. In particular, mass-based analytical methods show excellent sensitivity and precision for their quantification. This paper reviews recently published analytical methodologies for the sample preparation and for the determination of these compounds in different environmental and biological matrices by liquid chromatography coupled with mass spectrometry. The various sample preparation techniques are compared and discussed. In addition, recent developments and advances in this field are presented.

  7. Surface plasmon resonance based sensing of different chemical and biological samples using admittance loci method

    Science.gov (United States)

    Brahmachari, Kaushik; Ghosh, Sharmila; Ray, Mina

    2013-06-01

    The admittance loci method plays an important role in the design of multilayer thin film structures. In this paper, admittance loci method has been explored theoretically for sensing of various chemical and biological samples based on surface plasmon resonance (SPR) phenomenon. A dielectric multilayer structure consisting of a Boro silicate glass (BSG) substrate, calcium fluoride (CaF2) and zirconium dioxide (ZrO2) along with different dielectric layers has been investigated. Moreover, admittance loci as well as SPR curves of metal-dielectric multilayer structure consisting of the BSG substrate, gold metal film and various dielectric samples has been simulated in MATLAB environment. To validate the proposed simulation results, calibration curves have also been provided.

  8. Sample preparation for two-dimensional gel electrophoresis: considering the composition of biological material.

    Science.gov (United States)

    Knigge, Thomas; Letendre, Julie; Monsinjon, Tiphaine

    2013-11-01

    Comparative proteomic analyses in ecotoxicology and related fields require reproducible display of as many proteins as possible. In addition, it should be possible to carry out a quantitative comparison in a reliable manner. Sample preparation represents one of the essential steps toward these aims. In their work, Wu et al. describe how to deal with different recalcitrant tissues of varying species (Proteomics 2013, 13, 3205-3210). Their work underlines the necessity to adapt sample preparation to the specific requirements of the biological material. Beyond that Wu et al. present TRIzol® as feasible means for combined extraction of proteins and RNA. Indeed, using TRI-reagent extraction for proteomics, they resolve two problems at a time: that of removing contaminating compounds and that of simultaneous analysis of gene and protein expression. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Fiber laser-microscope system for femtosecond photodisruption of biological samples.

    Science.gov (United States)

    Yavaş, Seydi; Erdogan, Mutlu; Gürel, Kutan; Ilday, F Ömer; Eldeniz, Y Burak; Tazebay, Uygar H

    2012-03-01

    We report on the development of a ultrafast fiber laser-microscope system for femtosecond photodisruption of biological targets. A mode-locked Yb-fiber laser oscillator generates few-nJ pulses at 32.7 MHz repetition rate, amplified up to ∼125 nJ at 1030 nm. Following dechirping in a grating compressor, ∼240 fs-long pulses are delivered to the sample through a diffraction-limited microscope, which allows real-time imaging and control. The laser can generate arbitrary pulse patterns, formed by two acousto-optic modulators (AOM) controlled by a custom-developed field-programmable gate array (FPGA) controller. This capability opens the route to fine optimization of the ablation processes and management of thermal effects. Sample position, exposure time and imaging are all computerized. The capability of the system to perform femtosecond photodisruption is demonstrated through experiments on tissue and individual cells.

  10. The application of extraction chromatography to the determination of radionuclides in biological and environmental samples

    International Nuclear Information System (INIS)

    Testa, C.; Delle Site, A.

    1976-01-01

    The paper describe the application of extraction chromatography to the determination of several alpha and beta emitters in biological and environmental samples. Both column extraction chromatography and batch extraction process have been used to isolate the radionuclides from the samples. The effect of several parameters (extractant concentration, support granulometry, stirring time, temperature, presence of a complexing agent) on the extraction and elution has been examined. The application of redox extraction chromatography is also described. A very simple and rapid determination of the activity retained on the column can be obtained by transferring the slurry to a counting vial and by adding the scintillation liquid for a direct detection of the α or β emission. The counting efficiencies obtained with this technique are compared with those obtained with ion exchange resins. The organic polymers used for the extraction chromatography give about 100% counting efficiency. The conventional ion exchange resin cannot be used to this purpose because of their strong light absorption. (T.G.)

  11. ASPIRE: An automated sample positioning and irradiation system for radiation biology experiments at Inter University Accelerator Centre, New Delhi

    International Nuclear Information System (INIS)

    Kothari, Ashok; Barua, P.; Archunan, M.; Rani, Kusum; Subramanian, E.T.; Pujari, Geetanjali; Kaur, Harminder; Satyanarayanan, V.V.V.; Sarma, Asitikantha; Avasthi, D.K.

    2015-01-01

    An automated irradiation setup for biology samples has been built at Inter University Accelerator Centre (IUAC), New Delhi, India. It can automatically load and unload 20 biology samples in a run of experiment. It takes about 20 min [2% of the cell doubling time] to irradiate all the 20 samples. Cell doubling time is the time taken by the cells (kept in the medium) to grow double in numbers. The cells in the samples keep growing during entire of the experiment. The fluence irradiated to the samples is measured with two silicon surface barrier detectors. Tests show that the uniformity of fluence and dose of heavy ions reaches to 2% at the sample area in diameter of 40 mm. The accuracy of mean fluence at the center of the target area is within 1%. The irradiation setup can be used to the studies of radiation therapy, radiation dosimetry and molecular biology at the heavy ion accelerator. - Highlights: • Automated positioning and irradiation setup for biology samples at IUAC is built. • Loading and unloading of 20 biology samples can be automatically carried out. • Biologicals cells keep growing during entire experiment. • Fluence and dose of heavy ions are measured by two silicon barrier detectors. • Uniformity of fluence and dose of heavy ions at sample position reaches to 2%

  12. Separation and enrichment of trace ractopamine in biological samples by uniformly-sized molecularly imprinted polymers

    Directory of Open Access Journals (Sweden)

    Ya Li

    2012-12-01

    Full Text Available In order to prepare a high capacity packing material for solid-phase extraction with specific recognition ability of trace ractopamine in biological samples, uniformly-sized, molecularly imprinted polymers (MIPs were prepared by a multi-step swelling and polymerization method using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and toluene as a porogen respectively. Scanning electron microscope and specific surface area were employed to identify the characteristics of MIPs. Ultraviolet spectroscopy, Fourier transform infrared spectroscopy, Scatchard analysis and kinetic study were performed to interpret the specific recognition ability and the binding process of MIPs. The results showed that, compared with other reports, MIPs synthetized in this study showed high adsorption capacity besides specific recognition ability. The adsorption capacity of MIPs was 0.063 mmol/g at 1 mmol/L ractopamine concentration with the distribution coefficient 1.70. The resulting MIPs could be used as solid-phase extraction materials for separation and enrichment of trace ractopamine in biological samples. Keywords: Ractopamine, Uniformly-sized molecularly imprinted polymers, Solid-phase extraction, Multi-step swelling and polymerization, Separation and enrichment

  13. Separation and enrichment of trace ractopamine in biological samples by uniformly-sized molecularly imprinted polymers

    Science.gov (United States)

    Li, Ya; Fu, Qiang; Liu, Meng; Jiao, Yuan-Yuan; Du, Wei; Yu, Chong; Liu, Jing; Chang, Chun; Lu, Jian

    2012-01-01

    In order to prepare a high capacity packing material for solid-phase extraction with specific recognition ability of trace ractopamine in biological samples, uniformly-sized, molecularly imprinted polymers (MIPs) were prepared by a multi-step swelling and polymerization method using methacrylic acid as a functional monomer, ethylene glycol dimethacrylate as a cross-linker, and toluene as a porogen respectively. Scanning electron microscope and specific surface area were employed to identify the characteristics of MIPs. Ultraviolet spectroscopy, Fourier transform infrared spectroscopy, Scatchard analysis and kinetic study were performed to interpret the specific recognition ability and the binding process of MIPs. The results showed that, compared with other reports, MIPs synthetized in this study showed high adsorption capacity besides specific recognition ability. The adsorption capacity of MIPs was 0.063 mmol/g at 1 mmol/L ractopamine concentration with the distribution coefficient 1.70. The resulting MIPs could be used as solid-phase extraction materials for separation and enrichment of trace ractopamine in biological samples. PMID:29403774

  14. Expedient data mining for nontargeted high-resolution LC-MS profiles of biological samples.

    Science.gov (United States)

    Hnatyshyn, Serhiy; Shipkova, Petia; Sanders, Mark

    2013-05-01

    The application of high-resolution LC-MS metabolomics for drug candidate toxicity screening reflects phenotypic changes of an organism caused by induced chemical interferences. Its success depends not only on the ability to translate the acquired analytical information into biological knowledge, but also on the timely delivery of the results to aid the decision making process in drug discovery and development. Recent improvements in analytical instrumentation have resulted in the ability to acquire extremely information-rich datasets. These new data collection abilities have shifted the bottleneck in the timeline of metabolomic studies to the data analysis step. This paper describes our approach to expedient data analysis of nontargeted high-resolution LC-MS profiles of biological samples. The workflow is illustrated with the example of metabolomics study of time-dependent fasting in male rats. The results from measurement of 220 endogenous metabolites in urine samples illustrate significant biochemical changes induced by fasting. The developed software enables the reporting of relative quantities of annotated components while maintaining practical turnaround times. Each component annotation in the report is validated using both calculated isotopic peaks patterns and experimentally determined retention time data on standards.

  15. [The biomonitoring of toxic substances in biological samples of general population].

    Science.gov (United States)

    Ibarluzea, Jesús; Aurrekoetxea, Juan José; Porta, Miquel; Sunyer, Jordi; Ballester, Ferran

    2016-11-01

    Many of the world's most developed countries have adopted biomonitoring of toxic substances in order to ascertain their levels in biological samples. These substances get into the body through different environmental exposures. Monitoring toxic substances in biological samples should allow us to ascertain their levels in vulnerable groups, assess their evolution over time, make comparisons with levels observed in other countries, identify groups at risk or with high toxic levels and promote research. The main objective of biomonitoring is to act as a policy design tool to facilitate the implementation of particular measures in various sectors: health, environmental, agricultural and livestock or food industry sectors. In Spain, information on levels of toxic substances of environmental origin is provided by specific studies on health effects from environmental sources, such as the INMA project (INfancia y Medio Ambiente [childhood and environment]). In addition, biomonitoring projects have been implemented in Catalonia and the Canary Islands, together with a national biomonitoring programme in the adult working population. However, further progress is needed to develop a system that covers the general population as well as subgroups at risk, which relies on the collaboration of the involved authorities and the participation of professionals from different sectors and citizen organisations interested in the relationship between health and the environment. Copyright © 2016 SESPAS. Publicado por Elsevier España, S.L.U. All rights reserved.

  16. A comparison of quantitative reconstruction techniques for PIXE-tomography analysis applied to biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Beasley, D.G., E-mail: dgbeasley@ctn.ist.utl.pt [IST/C2TN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Alves, L.C. [IST/C2TN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Barberet, Ph.; Bourret, S.; Devès, G.; Gordillo, N.; Michelet, C. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Le Trequesser, Q. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Institut de Chimie de la Matière Condensée de Bordeaux (ICMCB, UPR9048) CNRS, Université de Bordeaux, 87 avenue du Dr. A. Schweitzer, Pessac F-33608 (France); Marques, A.C. [IST/IPFN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal); Seznec, H. [Univ. Bordeaux, CENBG, UMR 5797, F-33170 Gradignan (France); CNRS, IN2P3, CENBG, UMR 5797, F-33170 Gradignan (France); Silva, R.C. da [IST/IPFN, Universidade de Lisboa, Campus Tecnológico e Nuclear, E.N.10, 2686-953 Sacavém (Portugal)

    2014-07-15

    The tomographic reconstruction of biological specimens requires robust algorithms, able to deal with low density contrast and low element concentrations. At the IST/ITN microprobe facility new GPU-accelerated reconstruction software, JPIXET, has been developed, which can significantly increase the speed of quantitative reconstruction of Proton Induced X-ray Emission Tomography (PIXE-T) data. It has a user-friendly graphical user interface for pre-processing, data analysis and reconstruction of PIXE-T and Scanning Transmission Ion Microscopy Tomography (STIM-T). The reconstruction of PIXE-T data is performed using either an algorithm based on a GPU-accelerated version of the Maximum Likelihood Expectation Maximisation (MLEM) method or a GPU-accelerated version of the Discrete Image Space Reconstruction Algorithm (DISRA) (Sakellariou (2001) [2]). The original DISRA, its accelerated version, and the MLEM algorithm, were compared for the reconstruction of a biological sample of Caenorhabditis elegans – a small worm. This sample was analysed at the microbeam line of the AIFIRA facility of CENBG, Bordeaux. A qualitative PIXE-T reconstruction was obtained using the CENBG software package TomoRebuild (Habchi et al. (2013) [6]). The effects of pre-processing and experimental conditions on the elemental concentrations are discussed.

  17. Experience of an inter-laboratory exercise for the determination of Carbon-14 in biological samples

    International Nuclear Information System (INIS)

    Baburajan, A.; Rajaram, S.; D'Souza, Renita Shiny; Nayak, Rasmi; Karunakara, N.; Ravi, P.M.; Tripathi, R.M.

    2018-01-01

    Carbon-14 is one of the naturally occurring cosmogenic nuclide with long half life of 5730 y and beta energy, E max : 156 keV produced continuously in the outer atmosphere. It is also produced by the anthropogenic activities like nuclear weapon test, nuclear power plant etc. contributing to the atmospheric inventory. The 14 CO 2 gets incorporated with the plant species during photosynthesis and ultimately reaches to man through food chain. It is important to accurately quantify the level of 14 C in different biological matrices for the computation of radiation dose due to ingestion. There are different methods available for the determination of 14 C in biological samples. The oxidation of the dried sample is one of the methods used for liberating the 14 CO 2 and which in turn re-absorbed using Carbo Sorb and subjected to Liquid scintillation analyses with Permaflour scintillator solution. The paper deals with the quality assurance programme initiated by ESL, Tarapur along with ESL, Kalpakkam and CARER, Mangalore University and share the experience of the inter-laboratory comparison exercise

  18. Liquid chromatographic determination of CPZEN-45, a novel anti-tubercular drug, in biological samples.

    Science.gov (United States)

    Hanif, S N M; Hickey, A J; Garcia-Contreras, L

    2014-01-01

    CPZEN-45 is a new drug candidate being considered for the treatment of tuberculosis (TB). The aim of this study was to develop and validate a reverse-phase high-performance liquid chromatographic (HPLC) method suitable to determine CPZEN-45 concentrations in biological samples. CPZEN-45 was extracted from biological fluids and tissues (plasma, lung and spleen from guinea pig) by sequential extraction with acetonitrile and quantified by a Waters HPLC Alliance System coupled with a ZORBAX Bonus-RP column, guard column and UV detection at 263nm. The mobile phase was 20:80 acetonitrile:ultrapure-water with 0.05% TFA. The CPZEN-45 peak was eluted at 5.1min with no interference from the inherent peaks of plasma, bronchoalveolar lavage (BAL), lung or spleen tissues. Recovery of CPZEN-45 from biological samples was >96% of the spiked amount. The limit of detection was 0.05μg/ml and the limit of quantitation was 0.29μg/ml which was more than 5 and 21 times lower than the reported minimal inhibitory concentration of CPZEN-45 (MIC=1.56μg/ml for Mycobacterium tuberculosis and 6.25μg/ml for MDR-TB, respectively). Thus, HPLC method was deemed reliable, sensitive, reproducible and accurate for the determination of CPZEN-45 concentrations in plasma, BAL, lung and spleen tissues. Therefore, this method was used in subsequent studies in the guinea pig model to determine the disposition of CPZEN-45 after administration of solutions by the IV and SC routes. Copyright © 2013 Elsevier B.V. All rights reserved.

  19. An inexpensive and portable microvolumeter for rapid evaluation of biological samples.

    Science.gov (United States)

    Douglass, John K; Wcislo, William T

    2010-08-01

    We describe an improved microvolumeter (MVM) for rapidly measuring volumes of small biological samples, including live zooplankton, embryos, and small animals and organs. Portability and low cost make this instrument suitable for widespread use, including at remote field sites. Beginning with Archimedes' principle, which states that immersing an arbitrarily shaped sample in a fluid-filled container displaces an equivalent volume, we identified procedures that maximize measurement accuracy and repeatability across a broad range of absolute volumes. Crucial steps include matching the overall configuration to the size of the sample, using reflected light to monitor fluid levels precisely, and accounting for evaporation during measurements. The resulting precision is at least 100 times higher than in previous displacement-based methods. Volumes are obtained much faster than by traditional histological or confocal methods and without shrinkage artifacts due to fixation or dehydration. Calibrations using volume standards confirmed accurate measurements of volumes as small as 0.06 microL. We validated the feasibility of evaluating soft-tissue samples by comparing volumes of freshly dissected ant brains measured with the MVM and by confocal reconstruction.

  20. Rapid measurement of selenium in biological samples using instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    McKown, D.M.; Morris, J.S.

    1978-01-01

    A rapid instrumental system for measuring selenium via 17 second sup(77m)Se has been applied to the analysis of a wide variety of biological specimens encountered in biomedical research. Wet tissue specimens were lyophilized to remove water prior to analysis. Samples and standards were irradiated for 5 s at a thermal neutron flux of approximately 1x10 14 n.cm -2 .s -1 in the University of Missouri Research Reactor. The pneumatic transfer facility had a delivery time to the counting station of about 7 s. The returned shuttle rabbit was quickly opened and the sample vial transferred to a 45 cm 3 Ge(Li) detector gamma-ray spectrometer system. All samples were analyzed using a 5 s irradiation, 15 s decay, and 20 s count with a sample-to-detector distance giving less than 10% dead time at the analyzer. The clock time counting interval was measured to facilitete calculated correction for counting interval dead time if necessary. Gamma-ray spectra were recorded on computer compatible magnetic tape to facilitate data reduction using a modified version of the GAMANL spectrum analysis code. The reliability and versatility of the method is documented for serum and animal tissue specimens. Analysis results for SRM 1577 bovine liver show excellent accuracy and precision. (T.G.)

  1. Generator and Setup for Emulating Exposures of Biological Samples to Lightning Strokes.

    Science.gov (United States)

    Rebersek, Matej; Marjanovic, Igor; Begus, Samo; Pillet, Flavien; Rols, Marie-Pierre; Miklavcic, Damijan; Kotnik, Tadej

    2015-10-01

    We aimed to develop a system for controlled exposure of biological samples to conditions they experience when lightning strikes their habitats. We based the generator on a capacitor charged via a bridge rectifier and a dc-dc converter, and discharged via a relay, delivering arcs similar to natural lightning strokes in electric current waveform and similarly accompanied by acoustic shock waves. We coupled the generator to our exposure chamber described previously, measured electrical and acoustic properties of arc discharges delivered, and assessed their ability to inactivate bacterial spores. Submicrosecond discharges descended vertically from the conical emitting electrode across the air gap, entering the sample centrally and dissipating radially toward the ring-shaped receiving electrode. In contrast, longer discharges tended to short-circuit the electrodes. Recording at 341 000 FPS with Vision Research Phantom v2010 camera revealed that initial arc descent was still vertical, but became accompanied by arcs leaning increasingly sideways; after 8-12 μs, as the first of these arcs formed direct contact with the receiving electrode, it evolved into a channel of plasmified air and short-circuited the electrodes. We eliminated this artefact by incorporating an insulating cylinder concentrically between the electrodes, precluding short-circuiting between them. While bacterial spores are highly resistant to electric pulses delivered through direct contact, we showed that with arc discharges accompanied by an acoustic shock wave, spore inactivation is readily obtained. The presented system allows scientific investigation of effects of arc discharges on biological samples. This system will allow realistic experimental studies of lightning-triggered horizontal gene transfer and assessment of its role in evolution.

  2. Exploring Earth's Atmospheric Biology using a Platform-Extensible Sampling Payload

    Science.gov (United States)

    Gentry, D.; Rothschild, L.

    2012-12-01

    The interactions between Earth's atmosphere and its biosphere, or aerobiology, remain a significant unknown. What few studies have been done conclusively show that Earth's atmosphere has a rich and dynamic microbial presence[Bowers et al., 2010]; that microbes suspended in air survive over long times (1-2 weeks)[Smith et al., 2010] and travel great distances (>5000 km)[Kellogg and Griffin, 2006]; that some airborne bacteria actively nucleate ice crystals, affecting meteorology[Delort et al., 2010]; and that the presence of microbes in the atmosphere has other planetary-scale effects[Delort et al., 2010]. Basic questions, however, such as the number of microbes present, their activity level and state, the different species present and their variance over time and space, remain largely unquantified. Compounding the significant physical and environmental challenges of reliable aerobiological sampling, collection and analysis of biological samples at altitudes above ~10-20 km has traditionally used ad hoc instrumentation and techniques, yielding primarily qualitative analytical results that lack a common basis for comparison[Bowers et al., 2010]. There is a strong need for broad-basis, repeatable, reliably comparable data about aerobiological basics. We describe here a high-altitude environmental and biological sampling project designed specifically to address these issues. The goal is a robust, reliable, re-usable sampling system, with open reproducibility and adaptability for multiple low-cost flight platforms (including ground-tethered systems, high-altitude balloons, and suborbital sounding rockets); by establishing a common modular payload structure for high-altitude sampling with appeal to a broad user base, we hope to encourage widespread collection of comparable aerobiological data. We are on our third prototype iteration, with demonstrated function of two sample capture modules, a support backbone (tracking, data logging, event response, etc.), a simple ground

  3. Estimation of the fraction of biologically active methyl tert-butyl ether degraders in a heterogeneous biomass sample

    DEFF Research Database (Denmark)

    Waul, Christopher Kevin; Arvin, Erik; Schmidt, Jens Ejbye

    2008-01-01

    The fraction of biologically active methyl tert-butyl ether degraders in reactors is just as important for prediction of removal rates as knowledge of the kinetic parameters. The fraction of biologically active methyl tert-butyl ether degraders in a heterogeneous biomass sample, taken from a packed...

  4. Troubleshooting digital macro photography for image acquisition and the analysis of biological samples.

    Science.gov (United States)

    Liepinsh, Edgars; Kuka, Janis; Dambrova, Maija

    2013-01-01

    For years, image acquisition and analysis have been an important part of life science experiments to ensure the adequate and reliable presentation of research results. Since the development of digital photography and digital planimetric methods for image analysis approximately 20 years ago, new equipment and technologies have emerged, which have increased the quality of image acquisition and analysis. Different techniques are available to measure the size of stained tissue samples in experimental animal models of disease; however, the most accurate method is digital macro photography with software that is based on planimetric analysis. In this study, we described the methodology for the preparation of infarcted rat heart and brain tissue samples before image acquisition, digital macro photography techniques and planimetric image analysis. These methods are useful in the macro photography of biological samples and subsequent image analysis. In addition, the techniques that are described in this study include the automated analysis of digital photographs to minimize user input and exclude the risk of researcher-generated errors or bias during image analysis. Copyright © 2012 Elsevier Inc. All rights reserved.

  5. A validated HPTLC method for determination of terbutaline sulfate in biological samples: Application to pharmacokinetic study

    OpenAIRE

    Faiyazuddin, Md.; Rauf, Abdul; Ahmad, Niyaz; Ahmad, Sayeed; Iqbal, Zeenat; Talegaonkar, Sushma; Bhatnagar, Aseem; Khar, Roop K.; Ahmad, Farhan J.

    2011-01-01

    Terbutaline sulfate (TBS) was assayed in biological samples by validated HPTLC method. Densitometric analysis of TBS was carried out at 366 nm on precoated TLC aluminum plates with silica gel 60F254 as a stationary phase and chloroform–methanol (9.0:1.0, v/v) as a mobile phase. TBS was well resolved at RF 0.34 ± 0.02. In all matrices, the calibration curve appeared linear (r2 ⩾ 0.9943) in the tested range of 100–1000 ng spot−1 with a limit of quantification of 18.35 ng spot−1. Drug recovery f...

  6. Sensitivity and accuracy of atomic absorption spectrophotometry for trace elements in marine biological samples

    International Nuclear Information System (INIS)

    Fukai, R.; Oregioni, B.

    1976-01-01

    During the course of 1974-75 atomic absorption spectrophotometry (AAS) has been used extensively in our laboratory for measuring various trace elements in marine biological materials in order to conduct homogeneity tests on the intercalibration samples for trace metal analysis as well as to obtain baseline data for trace elements in various kinds of marine organisms collected from different locations in the Mediterranean Sea. Several series of test experiments have been conducted on the current methodology in use in our laboratory to ensure satisfactory analytical performance in measuring a number of trace elements for which analytical problems have not completely been solved. Sensitivities of the techniques used were repeatedly checked for various elements and the accuracy of the analyses were always critically evaluated by analyzing standard reference materials. The results of these test experiments have uncovered critical points relevant to the application of the AAS to routine analysis

  7. Use of self-actuating and self-sensing cantilevers for imaging biological samples in fluid.

    Science.gov (United States)

    Fantner, G E; Schumann, W; Barbero, R J; Deutschinger, A; Todorov, V; Gray, D S; Belcher, A M; Rangelow, I W; Youcef-Toumi, K

    2009-10-28

    In this paper, we present a detailed investigation into the suitability of atomic force microscopy (AFM) cantilevers with integrated deflection sensor and micro-actuator for imaging of soft biological samples in fluid. The Si cantilevers are actuated using a micro-heater at the bottom end of the cantilever. Sensing is achieved through p-doped resistors connected in a Wheatstone bridge. We investigated the influence of the water on the cantilever dynamics, the actuation and the sensing mechanisms, as well as the crosstalk between sensing and actuation. Successful imaging of yeast cells in water using the integrated sensor and actuator shows the potential of the combination of this actuation and sensing method. This constitutes a major step towards the automation and miniaturization required to establish AFM in routine biomedical diagnostics and in vivo applications.

  8. FIMic: design for ultimate 3D-integral microscopy of in-vivo biological samples.

    Science.gov (United States)

    Scrofani, G; Sola-Pikabea, J; Llavador, A; Sanchez-Ortiga, E; Barreiro, J C; Saavedra, G; Garcia-Sucerquia, J; Martínez-Corral, M

    2018-01-01

    In this work, Fourier integral microscope (FIMic), an ultimate design of 3D-integral microscopy, is presented. By placing a multiplexing microlens array at the aperture stop of the microscope objective of the host microscope, FIMic shows extended depth of field and enhanced lateral resolution in comparison with regular integral microscopy. As FIMic directly produces a set of orthographic views of the 3D-micrometer-sized sample, it is suitable for real-time imaging. Following regular integral-imaging reconstruction algorithms, a 2.75-fold enhanced depth of field and [Formula: see text]-time better spatial resolution in comparison with conventional integral microscopy is reported. Our claims are supported by theoretical analysis and experimental images of a resolution test target, cotton fibers, and in-vivo 3D-imaging of biological specimens.

  9. Determination of rhenium in biological and environmental samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Kucera, J.; Mizera, J.; Randa, Z.; Byrne, A.R.; Lucanikova, M.

    2006-01-01

    Radiochemical neutron activation procedures using liquid-liquid extraction with tetraphenylarsonium chloride in chloroform from 1 M HCl and solid extraction with ALIQUAT 336 incorporated in a polyacrylonitrile binding matrix from 0.1 M HCl were developed for accurate determination of rhenium in biological and environmental samples at the sub-ng.g -1 level. Concentrations of Re in the range of 0.1 to 2.4 ng.g -1 were determined in several botanical reference materials (RM), while in a RM of road dust a value of approx. 10 ng.g -1 was found. Significantly elevated values of Re, up to 90 ng.g -1 , were found in seaweed (brown algae). Results for Re in the brown algae Fucus vesiculosus in which elevated 99 Tc values had previously been determined suggest possible competition between Re and Tc in the accumulation process. (author)

  10. Lead levels in some biological samples of auto-mechanics in Abeokuta, Nigeria.

    Science.gov (United States)

    Babalola, O O; Ojo, L O; Aderemi, M O

    2005-12-01

    Lead levels were determined in the blood, scalp hair and fingernails of 38, all male auto-mechanics (aged 18-45 years) from Abeokuta, South-western Nigeria. The subjects were classified into four sub-groups based on the period of exposure namely: 1-5, 6-10, 11-15, and >16 years. Thirty-two occupationally unexposed subjects (mainly office workers) served as the control. The weight, height and body mass indexes of all subjects were noted, in addition to other information obtained through structured questionnaire. The mean values of blood lead (BPb), hair lead (HPb) and fingernail lead (NPb) of the occupationally exposed subjects (n=38) were 48.50 +/- 9.08 microg/dL, 17.75 +/- 5.16 microg/g, and 5.92 +/- 3.30 microg/g respectively, while the corresponding mean values for these parameters in the control subjects (n = 32) were 33.(,5 +/- 10.09 microg/dL, 14.30 +/- 5.90 microg/g and 5.31 +/- 2.77 microg/g respectively. The differences in BPb and HPb levels of the two groups were statistically significant (P <0.05 and P <0.01 respectively), while that of NPb was not significant. The levels of lead in the biological samples appeared to have no relationship with the number of years on the job. From these results, it was obvious that the higher levels of lead in the biological samples of test subjects, compared with those of the controls were from environmental sources.

  11. Microscopy of biological sample through advanced diffractive optics from visible to X-ray wavelength regime.

    Science.gov (United States)

    Di Fabrizio, Enzo; Cojoc, Dan; Emiliani, Valentina; Cabrini, Stefano; Coppey-Moisan, Maite; Ferrari, Enrico; Garbin, Valeria; Altissimo, Matteo

    2004-11-01

    The aim of this report is to demonstrate a unified version of microscopy through the use of advanced diffractive optics. The unified scheme derives from the technical possibility of realizing front wave engineering in a wide range of electromagnetic spectrum. The unified treatment is realized through the design and nanofabrication of phase diffractive elements (PDE) through which wave front beam shaping is obtained. In particular, we will show applications, by using biological samples, ranging from micromanipulation using optical tweezers to X-ray differential interference contrast (DIC) microscopy combined with X-ray fluorescence. We report some details on the design and physical implementation of diffractive elements that besides focusing also perform other optical functions: beam splitting, beam intensity, and phase redistribution or mode conversion. Laser beam splitting is used for multiple trapping and independent manipulation of micro-beads surrounding a cell as an array of tweezers and for arraying and sorting microscopic size biological samples. Another application is the Gauss to Laguerre-Gauss mode conversion, which allows for trapping and transfering orbital angular momentum of light to micro-particles immersed in a fluid. These experiments are performed in an inverted optical microscope coupled with an infrared laser beam and a spatial light modulator for diffractive optics implementation. High-resolution optics, fabricated by means of e-beam lithography, are demonstrated to control the intensity and the phase of the sheared beams in x-ray DIC microscopy. DIC experiments with phase objects reveal a dramatic increase in image contrast compared to bright-field x-ray microscopy. Besides the topographic information, fluorescence allows detection of certain chemical elements (Cl, P, Sc, K) in the same setup, by changing the photon energy of the x-ray beam. (c) 2005 Wiley-Liss, Inc.

  12. Cadmium determination in biological samples using neutron activation analysis with radiochemical separations

    International Nuclear Information System (INIS)

    Munoz A, Luis; Gras R, Nuri

    2005-01-01

    Chile has 7500 km of coastline on the Southern Pacific ocean,with about 4500 km of continental coastline that contains a variety of different geographical zones.This variety means that there is a great diversity of marine resources such as fish, shellfish and seaweeds. The utilization of these resources has been increasing in recent years making this sector an economically important one. The catch as of May 2002 came to 1.9 million tons and exports of the different species amounted to US$611.5 million as of April.But this important economic resource is being threatened by the technical demands imposed by importing countries, mainly the specific requirements for sanitary certification for fishery export products, depending on the markets of destination. The chemical element cadmium is one of the most strictly controlled elements due some shellfish accumulate a large amount of this element and to its high toxicity. The Chilean standard's analytical procedures for cadmium determination in hydro biological products, which must be met by laboratories that certify and control these products for export, are now being evaluated. Through its Chemical Metrology Unit, the Chilean Nuclear Energy Commission is strongly supporting this sector by preparing the secondary reference or control materials, and it has developed and implemented nuclear analytical methods for the certification of these materials, which will be used mostly in collaborative studies. This work describes the methodology developed for the determination of cadmium in biological samples, particularly in shellfish and fish. The method is based on neutron activation analysis with radiochemical separations, using the radioisotopes 115 Cd and 115m In, generated in the samples by bombarding with neutrons in a nuclear reactor. The samples were digested at 110 o C with H 2 SO 4 and H 2 O 2 and then the radioactive cadmium element was separated from the other elements present in the samples using a Bio Rad AG 2-X8

  13. Identification of cadmium in biological samples using neutron activation analysis with radiochemistry separations

    International Nuclear Information System (INIS)

    Munoz A, Luis; Gras R, Nuri

    2002-01-01

    Chile's 7500 km coastline of the Southern Pacific ocean, with about 4500 km of continental coastline that contains a variety of different geographical zones. This variety means that there is a great diversity of marine resources such as fish, shellfish and seaweeds. The utilization of these resources has been increasing in recent years making this sector an economically important one. The catch as of May 2002 came to 1.9 million tons and exports of the different species amounted to US$611.5 million as of April. But this important economic resource is being threatened by the technical demands imposed by importing countries, mainly the specific requirements for sanitary certification for fishery export products, depending on the markets of destination. The chemical element cadmium is one of the most strictly controlled elements due some shellfish accumulate a large amount of this element and to its high toxicity. The Chilean standard's analytical procedures for cadmium determination in hydro biological products, which must be met by laboratories that certify and control these products for export, are now being evaluated. Through its Chemical Metrology Unit, the Chilean Nuclear Energy Commission is strongly supporting this sector by preparing the secondary reference or control materials, and it has developed and implemented nuclear analytical methods for the certification of these materials, which will be used mostly in collaborative studies. This work describes the methodology developed for the determination of cadmium in biological samples, particularly in shellfish and fish. The method is based on neutron activation analysis with radiochemical separations, using the radioisotopes 115 Cd and 115m In, generated in the samples by bombarding with neutrons in a nuclear reactor. The samples were digested at 110 o C with H 2 SO 4 and H 2 O 2 and then the radioactive cadmium element was separated from the other elements present in the samples using a Bio Rad AG 2-X8 resin

  14. Determination of phosphorus and calcium in biological samples by activation with 14 MeV neutrons

    International Nuclear Information System (INIS)

    Berretta, Jose Roberto

    1995-01-01

    Analytical methods for phosphorus and calcium in biological samples by means of activation with 14 MeV neutrons, using the Van de Graaff accelerator from the Instituto de Pesquisas Energeticas e Nucleares, SP, Brazil are developed. For phosphorus analysis, powder samples were pressed into pellets, weighed and transferred to polyethylene plastic envelopes. The pellets with cadmium shielding were irradiated under a fast neutron flux for 5 to 10 minutes, and further counted in a HPGe detector for 5 minutes. Calcium analysis was performed by cyclic irradiation. Samples were irradiated for 10 minutes. After a decay time of 2 minutes, gamma counting was performed for 10 minutes. After a decay time of 2 minutes, a new irradiation ws made. The irradiation cycle was repeated 5 times and the counting spectrum obtained in each cycle was accumulated in the multi channel analyser. The variation of the neutron flux was followed by using a BF 3 detector calibrated with and aluminium monitor. By means of the gamma spectrum and the neutron counting of the BF 3 detector it was possible to estimate phosphorus and calcium concentrations in the sample analyzed. The methods were checked in the reference samples from the International Atomic Energy Agency and in commercial samples of powder milk, fertilizer and animal bone. Phosphorus contents in bone (A3/74) and milk (A-11) reference materials were (15.6 +- 1.8%) and (0.9 +- 0.1)%, respectively. These values are in good agreement to the certified values (15.5 +- 0.5)% and (0.910 +- 0.102)%, respectively. Calcium analysis carried out in bone (A3/74) presented a value of (31.8+-4.1)% and the certified value was of (31.3 +- 0.3)%. Detection limits for phosphorus and calcium were determined in different analyzed samples. The agreement of the results obtained with the certified values confirmed the suitability of the methods for phosphorus and calcium analysis. The methods are fast and laborious chemical procedures are not required. (author)

  15. Study on the determination of palladium in biological samples by the method of neutron activation analysis

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Queiroz

    2007-01-01

    Palladium is one of platinum group elements present in the nature at very low concentrations. However with the use of this element in the automobile catalyzers Pd became a new pollutant. Besides, Pd has been studied in the preparation of new antitumour drugs. Consequently, there is a need to determine Pd concentrations in biological and environmental samples. This study presents palladium results obtained in the analysis of biological samples and reference materials using instrumental thermal and epithermal neutron activation analysis (INAA and ENAA). The solvent extraction and solid phase extraction separation methods were also applied before ENAA. The samples analyzed in this study were, reference material BCR 723 - Palladium, Platinum and Rhodium in road dust, CCQM-P63 automotive catalyst material of the Proficiency Test and bovine tissue samples containing palladium prepared in the laboratory. Samples and palladium synthetic standard were irradiated at the IEA-R1 nuclear research reactor under thermal neutron flux of about 4 x 10 12 n cm-2 s-1, during a period of 4 and 16 h for INAA and ENAA, respectively. The induced gamma activity of 109 Pd to the sample and standard was measured using a hyper pure Ge detector coupled to a gamma ray spectrometer. The palladium concentration was calculated by comparative method. The gamma ray energy of 109 Pd radioisotope measured was of 88.0 keV, located in a spectrum region of low energy where occurs the interference of X rays, 'Bremsstrahlung' radiations, as well as Compton effect of 24 Na. The pre-separation of palladium from interfering elements by solvent extraction was performed using dimethylglyoxime complexant and chloroform as diluent. In the case of the pre separation procedure using solid reversed phase column, the palladium was retained using N,N-diethyl-N'-benzoyl thiourea complexant and eluted using ethanol. Aliquots of the resulting solutions from the pre-separations, free of interfering elements, were

  16. Biological Monitoring of Human Exposure to Neonicotinoids Using Urine Samples, and Neonicotinoid Excretion Kinetics.

    Science.gov (United States)

    Harada, Kouji H; Tanaka, Keiko; Sakamoto, Hiroko; Imanaka, Mie; Niisoe, Tamon; Hitomi, Toshiaki; Kobayashi, Hatasu; Okuda, Hiroko; Inoue, Sumiko; Kusakawa, Koichi; Oshima, Masayo; Watanabe, Kiyohiko; Yasojima, Makoto; Takasuga, Takumi; Koizumi, Akio

    2016-01-01

    Neonicotinoids, which are novel pesticides, have entered into usage around the world because they are selectively toxic to arthropods and relatively non-toxic to vertebrates. It has been suggested that several neonicotinoids cause neurodevelopmental toxicity in mammals. The aim was to establish the relationship between oral intake and urinary excretion of neonicotinoids by humans to facilitate biological monitoring, and to estimate dietary neonicotinoid intakes by Japanese adults. Deuterium-labeled neonicotinoid (acetamiprid, clothianidin, dinotefuran, and imidacloprid) microdoses were orally ingested by nine healthy adults, and 24 h pooled urine samples were collected for 4 consecutive days after dosing. The excretion kinetics were modeled using one- and two-compartment models, then validated in a non-deuterium-labeled neonicotinoid microdose study involving 12 healthy adults. Increased urinary concentrations of labeled neonicotinoids were observed after dosing. Clothianidin was recovered unchanged within 3 days, and most dinotefuran was recovered unchanged within 1 day. Around 10% of the imidacloprid dose was excreted unchanged. Most of the acetamiprid was metabolized to desmethyl-acetamiprid. Spot urine samples from 373 Japanese adults were analyzed for neonicotinoids, and daily intakes were estimated. The estimated average daily intake of these neonicotinoids was 0.53-3.66 μg/day. The highest intake of any of the neonicotinoids in the study population was 64.5 μg/day for dinotefuran, and this was <1% of the acceptable daily intake.

  17. Application of ion mobility spectrometry for the determination of tramadol in biological samples

    Directory of Open Access Journals (Sweden)

    Ali Sheibani

    2014-12-01

    Full Text Available In this study, a simple and rapid ion mobility spectrometry (IMS method has been described for the determination of tramadol. The operating instrumental parameters that could influence IMS were investigated and optimized (temperature; injection: 220 and IMS cell: 190°C, flow rate; carrier: 300 and drift: 600 mL/minute, voltage; corona: 2300 and drift: 7000 V, pulse width: 100 μs. Under optimum conditions, the calibration curves were linear within two orders of magnitude with R2 ≥ 0.998 for the determination of tramadol in human plasma, saliva, serum, and urine samples. The limits of detection and the limits of quantitation were between 0.1 and 0.3 and 0.3 and 1 ng/mL, respectively. The relative standard deviations were between 7.5 and 8.8%. The recovery results (90–103.9% indicate that the proposed method can be applied for tramadol analysis in different biological samples.

  18. Recent developments in HPLC analysis of β-blockers in biological samples.

    Science.gov (United States)

    Saleem, Kishwar; Ali, Imran; Kulsum, Umma; Aboul-Enein, Hassan Y

    2013-09-01

    β-Adrenergic blockers represent a very important class of drugs that are used worldwide for treating various cardiac diseases. The present article describes the state-of-the art of analyses of β-adrenergic blockers using high-performance liquid chromatography (HPLC). Sample preparation techniques such as liquid-liquid extraction, solid-phase extraction and solid-phase microextraction have been discussed, which are essential prior to HPLC analysis. Additionally, applications of liquid chromatography coupled with tandem mass spectrometry are included. HPLC methods have been reported to include 0.6-26 min as the run times and 0.01 ng/mL to 25 µg/mL as detection limits. The most commonly used columns were C18 with various buffers as the mobile phases, along with various organic modifiers. The optimization of HPLC conditions has been discussed. It has been observed that the reported methods are quite satisfactory for the analyses of β-adrenergic blockers in biological samples. Future perspectives in the hyphenation of solid-phase microextraction-nano-liquid chromatography-tandem mass spectrometry have also been highlighted to achieve detections at nanogram and picogram levels. The present article is very useful for academicians, scientists, drug and pharmaceutical personnel and government regulatory authorities.

  19. The correlation of arsenic levels in drinking water with the biological samples of skin disorders

    International Nuclear Information System (INIS)

    Kazi, Tasneem Gul; Arain, Muhammad Balal; Baig, Jameel Ahmed; Jamali, Muhammad Khan; Afridi, Hassan Imran; Jalbani, Nusrat; Sarfraz, Raja Adil; Shah, Abdul Qadir; Niaz, Abdul

    2009-01-01

    Arsenic (As) poisoning has become a worldwide public health concern. The skin is quite sensitive to As and skin lesions are the most common and earliest nonmalignant effects associated to chronic As exposure. In 2005-2007, a survey was carried out on surface and groundwater arsenic contamination and relationships between As exposure via the drinking water and related adverse health effects (melanosis and keratosis) on villagers resides on the banks of Manchar lake, southern part of Sindh, Pakistan. We screened the population from arsenic-affected villages, 61 to 73% population were identified patients suffering from chronic arsenic toxicity. The effects of As toxicity via drinking water were estimated by biological samples (scalp hair and blood) of adults (males and females), have or have not skin problem (n = 187). The referent samples of both genders were also collected from the areas having low level of As ( 2 = 0.852 and 0.718) as compared to non-diseased subjects (R 2 = 0.573 and 0.351), respectively

  20. Biological Monitoring of Human Exposure to Neonicotinoids Using Urine Samples, and Neonicotinoid Excretion Kinetics.

    Directory of Open Access Journals (Sweden)

    Kouji H Harada

    Full Text Available Neonicotinoids, which are novel pesticides, have entered into usage around the world because they are selectively toxic to arthropods and relatively non-toxic to vertebrates. It has been suggested that several neonicotinoids cause neurodevelopmental toxicity in mammals. The aim was to establish the relationship between oral intake and urinary excretion of neonicotinoids by humans to facilitate biological monitoring, and to estimate dietary neonicotinoid intakes by Japanese adults.Deuterium-labeled neonicotinoid (acetamiprid, clothianidin, dinotefuran, and imidacloprid microdoses were orally ingested by nine healthy adults, and 24 h pooled urine samples were collected for 4 consecutive days after dosing. The excretion kinetics were modeled using one- and two-compartment models, then validated in a non-deuterium-labeled neonicotinoid microdose study involving 12 healthy adults. Increased urinary concentrations of labeled neonicotinoids were observed after dosing. Clothianidin was recovered unchanged within 3 days, and most dinotefuran was recovered unchanged within 1 day. Around 10% of the imidacloprid dose was excreted unchanged. Most of the acetamiprid was metabolized to desmethyl-acetamiprid. Spot urine samples from 373 Japanese adults were analyzed for neonicotinoids, and daily intakes were estimated. The estimated average daily intake of these neonicotinoids was 0.53-3.66 μg/day. The highest intake of any of the neonicotinoids in the study population was 64.5 μg/day for dinotefuran, and this was <1% of the acceptable daily intake.

  1. Biological Monitoring of Human Exposure to Neonicotinoids Using Urine Samples, and Neonicotinoid Excretion Kinetics

    Science.gov (United States)

    Harada, Kouji H.; Tanaka, Keiko; Sakamoto, Hiroko; Imanaka, Mie; Niisoe, Tamon; Hitomi, Toshiaki; Kobayashi, Hatasu; Okuda, Hiroko; Inoue, Sumiko; Kusakawa, Koichi; Oshima, Masayo; Watanabe, Kiyohiko; Yasojima, Makoto; Takasuga, Takumi; Koizumi, Akio

    2016-01-01

    Background Neonicotinoids, which are novel pesticides, have entered into usage around the world because they are selectively toxic to arthropods and relatively non-toxic to vertebrates. It has been suggested that several neonicotinoids cause neurodevelopmental toxicity in mammals. The aim was to establish the relationship between oral intake and urinary excretion of neonicotinoids by humans to facilitate biological monitoring, and to estimate dietary neonicotinoid intakes by Japanese adults. Methodology/Principal Findings Deuterium-labeled neonicotinoid (acetamiprid, clothianidin, dinotefuran, and imidacloprid) microdoses were orally ingested by nine healthy adults, and 24 h pooled urine samples were collected for 4 consecutive days after dosing. The excretion kinetics were modeled using one- and two-compartment models, then validated in a non-deuterium-labeled neonicotinoid microdose study involving 12 healthy adults. Increased urinary concentrations of labeled neonicotinoids were observed after dosing. Clothianidin was recovered unchanged within 3 days, and most dinotefuran was recovered unchanged within 1 day. Around 10% of the imidacloprid dose was excreted unchanged. Most of the acetamiprid was metabolized to desmethyl-acetamiprid. Spot urine samples from 373 Japanese adults were analyzed for neonicotinoids, and daily intakes were estimated. The estimated average daily intake of these neonicotinoids was 0.53–3.66 μg/day. The highest intake of any of the neonicotinoids in the study population was 64.5 μg/day for dinotefuran, and this was <1% of the acceptable daily intake. PMID:26731104

  2. An efficient and sensitive method for preparing cDNA libraries from scarce biological samples.

    Science.gov (United States)

    Sterling, Catherine H; Veksler-Lublinsky, Isana; Ambros, Victor

    2015-01-01

    The preparation and high-throughput sequencing of cDNA libraries from samples of small RNA is a powerful tool to quantify known small RNAs (such as microRNAs) and to discover novel RNA species. Interest in identifying the small RNA repertoire present in tissues and in biofluids has grown substantially with the findings that small RNAs can serve as indicators of biological conditions and disease states. Here we describe a novel and straightforward method to clone cDNA libraries from small quantities of input RNA. This method permits the generation of cDNA libraries from sub-picogram quantities of RNA robustly, efficiently and reproducibly. We demonstrate that the method provides a significant improvement in sensitivity compared to previous cloning methods while maintaining reproducible identification of diverse small RNA species. This method should have widespread applications in a variety of contexts, including biomarker discovery from scarce samples of human tissue or body fluids. © The Author(s) 2014. Published by Oxford University Press on behalf of Nucleic Acids Research.

  3. Bias in tensor based morphometry Stat-ROI measures may result in unrealistic power estimates.

    Science.gov (United States)

    Thompson, Wesley K; Holland, Dominic

    2011-07-01

    A series of reports have recently appeared using tensor based morphometry statistically-defined regions of interest, Stat-ROIs, to quantify longitudinal atrophy in structural MRIs from the Alzheimer's Disease Neuroimaging Initiative (ADNI). This commentary focuses on one of these reports, Hua et al. (2010), but the issues raised here are relevant to the others as well. Specifically, we point out a temporal pattern of atrophy in subjects with Alzheimer's disease and mild cognitive impairment whereby the majority of atrophy in two years occurs within the first 6 months, resulting in overall elevated estimated rates of change. Using publicly-available ADNI data, this temporal pattern is also found in a group of identically-processed healthy controls, strongly suggesting that methodological bias is corrupting the measures. The resulting bias seriously impacts the validity of conclusions reached using these measures; for example, sample size estimates reported by Hua et al. (2010) may be underestimated by a factor of five to sixteen. Copyright © 2011 Elsevier Inc. All rights reserved.

  4. Methods for the physical characterization and quantification of extracellular vesicles in biological samples.

    Science.gov (United States)

    Rupert, Déborah L M; Claudio, Virginia; Lässer, Cecilia; Bally, Marta

    2017-01-01

    Our body fluids contain a multitude of cell-derived vesicles, secreted by most cell types, commonly referred to as extracellular vesicles. They have attracted considerable attention for their function as intercellular communication vehicles in a broad range of physiological processes and pathological conditions. Extracellular vesicles and especially the smallest type, exosomes, have also generated a lot of excitement in view of their potential as disease biomarkers or as carriers for drug delivery. In this context, state-of-the-art techniques capable of comprehensively characterizing vesicles in biological fluids are urgently needed. This review presents the arsenal of techniques available for quantification and characterization of physical properties of extracellular vesicles, summarizes their working principles, discusses their advantages and limitations and further illustrates their implementation in extracellular vesicle research. The small size and physicochemical heterogeneity of extracellular vesicles make their physical characterization and quantification an extremely challenging task. Currently, structure, size, buoyant density, optical properties and zeta potential have most commonly been studied. The concentration of vesicles in suspension can be expressed in terms of biomolecular or particle content depending on the method at hand. In addition, common quantification methods may either provide a direct quantitative measurement of vesicle concentration or solely allow for relative comparison between samples. The combination of complementary methods capable of detecting, characterizing and quantifying extracellular vesicles at a single particle level promises to provide new exciting insights into their modes of action and to reveal the existence of vesicle subpopulations fulfilling key biological tasks. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Quantification of Hg excretion and distribution in biological samples of mercury-dental-amalgam users and its correlation with biological variables.

    Science.gov (United States)

    Gul, Nayab; Khan, Sardar; Khan, Abbas; Nawab, Javed; Shamshad, Isha; Yu, Xinwei

    2016-10-01

    This is the first study conducted to quantify the excretion and distribution of mercury (Hg) with time (days) in the biological samples collected from Hg dental amalgam users (MDA). The individuals, with Hg-based dental filling were selected, and their biological samples (red blood cells (RBCs), plasma, urine, hair, and nails) were collected on first, third, and 12th day of fillings. The concentrations of Hg observed in the biological samples of MDA were also correlated with the biological variables such as age, weight, restoration, fish consumption, number, and surface area of fillings. The concentrations of Hg in the biological samples of MDA were found 6-8 times higher than the non-amalgam users (control). The concentrations of Hg in the RBCs (4.39 μg/L), plasma (3.02 μg/L), and urine (22.5 μg/L) on first day of filling were found comparatively higher than the concentrations observed on third day (2.15, 1.46, and 12.3 μg/L for RBCs, plasma, urine, respectively) and 12th day (3.05, 2.5, 9.12 μg/L for RBCs, plasma, urine, respectively), while Hg concentrations were found lower in the hair and nails on third day of fillings (1.53 μg/g for hair and 2.35 μg/g for nails) as compared to the 12th day (2.95 μg/g for hair and 3.5 μg/g for nails). The correlations were found significant (p ˂ 0.05) between Hg concentrations in the biological samples of MDA and biological variables (the number of restoration, fish consumption, number, and surface area of fillings), while no significant (p ˃ 0.05) correlations were observed for Hg concentrations in the biological samples with age and weight of MDA. These observations unveil the fact that the use of Hg-based dental filling is the undesirable exposure to Hg which should be replaced by composite (a safer filling material).

  6. Nanoparticle sensor for label free detection of swine DNA in mixed biological samples

    International Nuclear Information System (INIS)

    Ali, M E; Hashim, U; Mustafa, S; Che Man, Y B; Yusop, M H M; Bari, M F; Islam, Kh N; Hasan, M F

    2011-01-01

    We used 40 ± 5 nm gold nanoparticles (GNPs) as colorimetric sensor to visually detect swine-specific conserved sequence and nucleotide mismatch in PCR-amplified and non-amplified mitochondrial DNA mixtures to authenticate species. Colloidal GNPs changed color from pinkish-red to gray-purple in 2 mM PBS. Visually observed results were clearly reflected by the dramatic reduction of surface plasmon resonance peak at 530 nm and the appearance of new features in the 620-800 nm regions in their absorption spectra. The particles were stabilized against salt-induced aggregation upon the adsorption of single-stranded DNA. The PCR products, without any additional processing, were hybridized with a 17-base probe prior to exposure to GNPs. At a critical annealing temperature (55 0 C) that differentiated matched and mismatched base pairing, the probe was hybridized to pig PCR product and dehybridized from the deer product. The dehybridized probe stuck to GNPs to prevent them from salt-induced aggregation and retained their characteristic red color. Hybridization of a 27-nucleotide probe to swine mitochondrial DNA identified them in pork-venison, pork-shad and venison-shad binary admixtures, eliminating the need of PCR amplification. Thus the assay was applied to authenticate species both in PCR-amplified and non-amplified heterogeneous biological samples. The results were determined visually and validated by absorption spectroscopy. The entire assay (hybridization plus visual detection) was performed in less than 10 min. The LOD (for genomic DNA) of the assay was 6 μg ml -1 swine DNA in mixed meat samples. We believe the assay can be applied for species assignment in food analysis, mismatch detection in genetic screening and homology studies between closely related species.

  7. Nanoparticle sensor for label free detection of swine DNA in mixed biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Ali, M E; Hashim, U [Institute of Nano Electronic Engineering (INNE), Universiti Malaysia Perlis, Lot 104-108, Tingkat 1, Block A, Taman Pertiwi Indah, Jalan Kangar-Alor Star, Seriab, 01000 Kangar, Perlis (Malaysia); Mustafa, S; Che Man, Y B; Yusop, M H M [Halal Products Research Institute, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Bari, M F [School of Materials Engineering, University Malaysia Perlis, Seriab 01000, Kangar, Perlis (Malaysia); Islam, Kh N [Department of Preclinical Sciences, Faculty of Veterinary Medicine, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia); Hasan, M F, E-mail: uda@unimap.edu.my [Department of Crop Science, Faculty of Agriculture, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor (Malaysia)

    2011-05-13

    We used 40 {+-} 5 nm gold nanoparticles (GNPs) as colorimetric sensor to visually detect swine-specific conserved sequence and nucleotide mismatch in PCR-amplified and non-amplified mitochondrial DNA mixtures to authenticate species. Colloidal GNPs changed color from pinkish-red to gray-purple in 2 mM PBS. Visually observed results were clearly reflected by the dramatic reduction of surface plasmon resonance peak at 530 nm and the appearance of new features in the 620-800 nm regions in their absorption spectra. The particles were stabilized against salt-induced aggregation upon the adsorption of single-stranded DNA. The PCR products, without any additional processing, were hybridized with a 17-base probe prior to exposure to GNPs. At a critical annealing temperature (55 {sup 0}C) that differentiated matched and mismatched base pairing, the probe was hybridized to pig PCR product and dehybridized from the deer product. The dehybridized probe stuck to GNPs to prevent them from salt-induced aggregation and retained their characteristic red color. Hybridization of a 27-nucleotide probe to swine mitochondrial DNA identified them in pork-venison, pork-shad and venison-shad binary admixtures, eliminating the need of PCR amplification. Thus the assay was applied to authenticate species both in PCR-amplified and non-amplified heterogeneous biological samples. The results were determined visually and validated by absorption spectroscopy. The entire assay (hybridization plus visual detection) was performed in less than 10 min. The LOD (for genomic DNA) of the assay was 6 {mu}g ml{sup -1} swine DNA in mixed meat samples. We believe the assay can be applied for species assignment in food analysis, mismatch detection in genetic screening and homology studies between closely related species.

  8. Fast screening of ketamine in biological samples based on molecularly imprinted photonic hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Liang [Department of Forensic Science, People' s Public Security University of China, Beijing (China); Meng, Pinjia, E-mail: mengpinjia@163.com [Department of Forensic Science, People' s Public Security University of China, Beijing (China); Zhang, Qingqing; Wang, Yanji [Department of Forensic Science, People' s Public Security University of China, Beijing (China)

    2013-04-10

    Graphical abstract: A novel label-free colorimetric chemosensor: with the increase in the concentration of ketamine, the Bragg diffraction peak of MIPHs gradually shifted to the longer wavelength region. Accompanying the peak shift, the color change of MIPHs was also observed obviously: from green to red. Highlights: ► We developed the label-free colorimetric MIPHs for handy and fast screening of ketamine. ► The obvious color change of MIPHs was observed upon ketamine. ► The MIPHs exhibited good sensing abilities in an aqueous environment. ► The sensing mechanisms of the water-compatible MIPHs were investigated. ► The MIPHs were employed to screening ketamine in real biological samples. -- Abstract: A novel label-free colorimetric chemosensor was developed for handy and fast screening of ketamine with high sensitivity and specificity based on molecularly imprinted photonic hydrogels (MIPHs) that combined the colloidal-crystal with molecular imprinting technique. The unique inverse opal arrays with a thin polymer wall in which the imprinted nanocavities of ketamine moleculars distributed allowed high sensitive, quick responsive, specific detection of the target analyte, and good regenerating ability in an aqueous environment. Due to the hierarchical inverse opal structural characteristics, the specific ketamine molecular recognition process can induce obvious swelling of the MIPHs to be directly transferred into visually perceptible optical signal (change in color) which can be detected by the naked eye through Bragg diffractive shifts of ordered macroporous arrays. In order to enhance the recognition ability in aqueous environments, the MIPHs were designed as water-compatible and synthesized in a water–methanol system. The molecular recognition mechanisms were investigated. The proposed MIPHs were successfully employed to screen trace level ketamine in human urine and saliva samples, exhibiting high sensitivity, rapid response, and specificity in the

  9. Mass amplifying probe for sensitive fluorescence anisotropy detection of small molecules in complex biological samples.

    Science.gov (United States)

    Cui, Liang; Zou, Yuan; Lin, Ninghang; Zhu, Zhi; Jenkins, Gareth; Yang, Chaoyong James

    2012-07-03

    detection of small molecules by means of FA in complex biological samples.

  10. Development of novel separation techniques for biological samples in capillary electrophoresis

    Energy Technology Data Exchange (ETDEWEB)

    Chang, Huan -Tsung [Iowa State Univ., Ames, IA (United States)

    1994-07-27

    This dissertation includes three different topics: general introduction of capillary electrophoresis (CE); gradient in CE and CE in biological separations; and capillary gel electrophoresis (CGE) for DNA separation. Factors such as temperature, viscosity, pH, and the surface of capillary walls affecting the separation performance are demonstrated. A pH gradient between 3.0 and 5.2 is useful to improve the resolution among eight different organic acids. A flow gradient due to the change in the concentration of surfactant, which is able to coat to the capillary wall to change the flow rate and its direction, is also shown as a good way to improve the resolution for organic compounds. A temperature gradient caused by joule heat is shown by voltage programming to enhance the resolution and shorten the separation time for several phenolic compounds. The author also shows that self-regulating dynamic control of electroosmotic flow in CE by simply running separation in different concentrations of surfactant has less matrix effect on the separation performance. One of the most important demonstrations in this dissertation is that the author proposes on-column reaction which gives several advantages including the use of a small amount of sample, low risk of contamination, and time saving and kinetic features. The author uses this idea with laser induced fluorescence (LIF) as a detection mode to detect an on-column digestion of sub-ng of protein. This technique also is applied to single cell analysis in the group.

  11. Synthesis of [13C6]-labelled phenethylamine derivatives for drug quantification in biological samples.

    Science.gov (United States)

    Karlsen, Morten; Liu, HuiLing; Berg, Thomas; Johansen, Jon Eigill; Hoff, Bård Helge

    2014-05-15

    The availability of high-quality (13)C-labelled internal standards will improve accurate quantification of narcotics and drugs in biological samples. Thus, the synthesis of 10 [(13)C6]-labelled phenethylamine derivatives, namely amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, 3,4-methylenedioxy-N-ethylamphetamine, 4-methoxyamphetamine, 4-methoxymethamphetamine, 3,5-dimethoxyphenethylamine 4-bromo-2,5-dimethoxyphenethylamine and 2,5-dimethoxy-4-iodophenethylamine, have been undertaken. [(13)C6]-Phenol proved to be an excellent starting material for making (13)C-labelled narcotic substances in the phenethylamine class, and a developed Stille-type coupling enabled an efficient synthesis of the 3,4-methylenedioxy and 4-methoxy derivatives. The pros and cons of alternative routes and transformations are also discussed. The [(13)C6]-labelled compounds are intended for use as internal standards in forensic analysis, health sciences and metabolomics studies by gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry. Copyright © 2014 John Wiley & Sons, Ltd.

  12. Simple and sensitive determination of sparfloxacin in pharmaceuticals and biological samples by immunoassay

    Directory of Open Access Journals (Sweden)

    Hua-Jin Zeng

    2012-06-01

    Full Text Available Plasma quinolone concentrations are not routinely measured in clinical practice. However, in order to optimize quinolone treatment, monitoring of plasma concentrations could sometimes be useful particularly in critically ill patients. In this study, anti-sparfloxacin antibody was obtained by immunizing rabbits with sparfloxacin conjugated with bovine serum albumin using isobutyl chloroformate method. After the assay procedure was optimized, the standard curve of sparfloxacin was established. The practical measuring range of the competitive ELISA extended from 5 ng/mL to 2 μg/mL. The recovery rates and coefficients of variation for rat plasma, urine and tissues were 87.7–106.2% and 4.8–15.3%, respectively. To demonstrate the potential of the ELISA, a preliminary pharmacokinetics and tissue distribution study of sparfloxacin in rats and quantitative analysis of sparfloxacin in several pharmaceuticals were performed and compared with high-performance liquid chromatography (HPLC. The experimental data indicated that the proposed method would be a valuable tool in therapeutic drug monitoring (TDM for sparfloxacin. Keywords: Sparfloxacin, Enzyme-linked immunosorbent assay (ELISA, Biological samples, Pharmacokinetics, Tissue distribution

  13. Development of a new catalase activity assay for biological samples using optical CUPRAC sensor

    Science.gov (United States)

    Bekdeşer, Burcu; Özyürek, Mustafa; Güçlü, Kubilay; Alkan, Fulya Üstün; Apak, Reşat

    2014-11-01

    A novel catalase activity assay was developed for biological samples (liver and kidney tissue homogenates) using a rapid and low-cost optical sensor-based ‘cupric reducing antioxidant capacity' (CUPRAC) method. The reagent, copper(II)-neocuproine (Cu(II)-Nc) complex, was immobilized onto a cation-exchanger film of Nafion, and the absorbance changes associated with the formation of the highly-colored Cu(I)-Nc chelate as a result of reaction with hydrogen peroxide (H2O2) was measured at 450 nm. When catalase was absent, H2O2 produced the CUPRAC chromophore, whereas catalase, being an effective H2O2 scavenger, completely annihilated the CUPRAC signal due to H2O2. Thus, the CUPRAC absorbance due to H2O2 oxidation concomitant with Cu(I)-Nc formation decreased proportionally with catalase. The developed sensor gave a linear response over a wide concentration range of H2O2 (0.68-78.6 μM). This optical sensor-based method applicable to tissue homogenates proved to be efficient for low hydrogen peroxide concentrations (physiological and nontoxic levels) to which the widely used UV method is not accurately responsive. Thus, conventional problems of the UV method arising from relatively low sensitivity and selectivity, and absorbance disturbance due to gaseous oxygen evolution were overcome. The catalase findings of the proposed method for tissue homogenates were statistically alike with those of HPLC.

  14. Development of a new catalase activity assay for biological samples using optical CUPRAC sensor.

    Science.gov (United States)

    Bekdeşer, Burcu; Özyürek, Mustafa; Güçlü, Kubilay; Alkan, Fulya Üstün; Apak, Reşat

    2014-11-11

    A novel catalase activity assay was developed for biological samples (liver and kidney tissue homogenates) using a rapid and low-cost optical sensor-based 'cupric reducing antioxidant capacity' (CUPRAC) method. The reagent, copper(II)-neocuproine (Cu(II)-Nc) complex, was immobilized onto a cation-exchanger film of Nafion, and the absorbance changes associated with the formation of the highly-colored Cu(I)-Nc chelate as a result of reaction with hydrogen peroxide (H2O2) was measured at 450 nm. When catalase was absent, H2O2 produced the CUPRAC chromophore, whereas catalase, being an effective H2O2 scavenger, completely annihilated the CUPRAC signal due to H2O2. Thus, the CUPRAC absorbance due to H2O2 oxidation concomitant with Cu(I)-Nc formation decreased proportionally with catalase. The developed sensor gave a linear response over a wide concentration range of H2O2 (0.68-78.6 μM). This optical sensor-based method applicable to tissue homogenates proved to be efficient for low hydrogen peroxide concentrations (physiological and nontoxic levels) to which the widely used UV method is not accurately responsive. Thus, conventional problems of the UV method arising from relatively low sensitivity and selectivity, and absorbance disturbance due to gaseous oxygen evolution were overcome. The catalase findings of the proposed method for tissue homogenates were statistically alike with those of HPLC. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. The method of radioactive tracer for measuring the amount of inorganic nanoparticles in biological samples

    Science.gov (United States)

    Buzulukov, Yu; Antsiferova, A.; Demin, V. A.; Demin, V. F.; Kashkarov, P.

    2015-11-01

    The method to measure the mass of inorganic nanoparticles in biological (or any other samples) using nanoparticles labeled with radioactive tracers is developed and applied to practice. The tracers are produced in original nanoparticles by radioactive activation of some of their atomic nuclei. The method of radioactive tracers demonstrates a sensitivity, specificity and accuracy equal or better than popular methods of optical and mass spectrometry, or electron microscopy and has some specific advantages. The method can be used for study of absorption, distribution, metabolism and excretion in living organism, as well as in ecological and fundamental research. It was used in practice to study absorption, distribution, metabolism and excretion of nanoparticles of Ag, Au, Se, ZnO, TiO2 as well as to study transportation of silver nanoparticles through the barriers of blood-brain, placenta and milk gland of rats. Brief descriptions of data obtained in experiments with application of this method included in the article. The method was certified in Russian Federation standard system GOST-R and recommended by the Russian Federation regulation authority ROSPOTREBNADZOR for measuring of toxicokinetic and organotropy parameters of nanoparticles.

  16. Substrate-zymography: a still worthwhile method for gelatinases analysis in biological samples.

    Science.gov (United States)

    Ricci, Serena; D'Esposito, Vittoria; Oriente, Francesco; Formisano, Pietro; Di Carlo, Angelina

    2016-08-01

    Matrix metallo-proteinases (MMPs) are a family of zinc-dependent endopeptidases, capable of degrading all the molecular components of extracellular matrix. A class of MMPs is gelatinases which includes gelatinase A or MMP-2 (72 kDa) and gelatinase B or MMP-9 (92 kDa), which have been shown to play critical roles in pathophysiology of many human disease and, in particular, cancer progression. For these reasons they obtained a great interest as potential non-invasive biomarker in providing useful clinical information in cancer diagnosis and therapy. A sensitive and unexpensive method for analysis of gelatinases is the gelatine zymography, which allows to measure the relative amounts of active and inactive enzymes in body fluids and tissue extracts. The procedure involves the electrophoretic separation of proteins under denaturing but non reducing conditions through a polyacrylamide gel containing a synthetic substrate (gelatin). The aim of this mini-review has been to describe the general principles of gelatine zymography technique, underling the main advantages and disadvantages. Even though an improvement of this method is necessary for a better applicability in laboratory medicine, gelatine zymography represents the most convenient method to detect the activity of the different gelatinases from a wide range of biological samples.

  17. Unbiased Rare Event Sampling in Spatial Stochastic Systems Biology Models Using a Weighted Ensemble of Trajectories.

    Directory of Open Access Journals (Sweden)

    Rory M Donovan

    2016-02-01

    Full Text Available The long-term goal of connecting scales in biological simulation can be facilitated by scale-agnostic methods. We demonstrate that the weighted ensemble (WE strategy, initially developed for molecular simulations, applies effectively to spatially resolved cell-scale simulations. The WE approach runs an ensemble of parallel trajectories with assigned weights and uses a statistical resampling strategy of replicating and pruning trajectories to focus computational effort on difficult-to-sample regions. The method can also generate unbiased estimates of non-equilibrium and equilibrium observables, sometimes with significantly less aggregate computing time than would be possible using standard parallelization. Here, we use WE to orchestrate particle-based kinetic Monte Carlo simulations, which include spatial geometry (e.g., of organelles, plasma membrane and biochemical interactions among mobile molecular species. We study a series of models exhibiting spatial, temporal and biochemical complexity and show that although WE has important limitations, it can achieve performance significantly exceeding standard parallel simulation--by orders of magnitude for some observables.

  18. Method development for mass spectrometry based molecular characterization of fossil fuels and biological samples

    Science.gov (United States)

    Mahat, Rajendra K.

    In an analytical (chemical) method development process, the sample preparation step usually determines the throughput and overall success of the analysis. Both targeted and non-targeted methods were developed for the mass spectrometry (MS) based analyses of fossil fuels (coal) and lipidomic analyses of a unique micro-organism, Gemmata obscuriglobus. In the non-targeted coal analysis using GC-MS, a microwave-assisted pressurized sample extraction method was compared with the traditional extraction method, such as Soxhlet. On the other hand, methods were developed to establish a comprehensive lipidomic profile and to confirm the presence of endotoxins (a.k.a. lipopolysaccharides, LPS) in Gemmata.. The performance of pressurized heating techniques employing hot-air oven and microwave irradiation were compared with that of Soxhlet method in terms of percentage extraction efficiency and extracted analyte profiles (via GC-MS). Sub-bituminous (Powder River Range, Wyoming, USA) and bituminous (Fruitland formation, Colorado, USA) coal samples were tested. Overall 30-40% higher extraction efficiencies (by weight) were obtained with a 4 hour hot-air oven and a 20 min microwave-heating extraction in a pressurized container when compared to a 72 hour Soxhlet extraction. The pressurized methods are 25 times more economic in terms of solvent/sample amount used and are 216 times faster in term of time invested for the extraction process. Additionally, same sets of compounds were identified by GC-MS for all the extraction methods used: n-alkanes and diterpanes in the sub-bituminous sample, and n-alkanes and alkyl aromatic compounds in the bituminous coal sample. G. obscuriglobus, a nucleated bacterium, is a micro-organism of high significances from evolutionary, cell and environmental biology standpoints. Although lipidomics is an essential tool in microbiological systematics and chemotaxonomy, complete lipid profile of this bacterium is still lacking. In addition, the presence of

  19. Metais pesados em amostras biológicas de bovinos Heavy metals in cattle biological samples

    Directory of Open Access Journals (Sweden)

    Maria Verônica de Souza

    2009-09-01

    Full Text Available O objetivo deste trabalho foi determinar a concentração de metais pesados no sangue (Pb, Ni e Cd, soro (Cu e Zn, pelo e leite (Pb, Ni, Cd, Cu e Zn de bovinos criados em área industrializada (com siderúrgicas e não-industrial do Estado de Minas Gerais, em amostras coletadas em duas épocas (inverno e verão, buscando avaliar a contaminação em animais em função do ambiente de exposição e da estação do ano. O local de criação dos animais afetou significativamente somente a concentração de Cu obtida nas amostras de soro, com maiores valores determinados no grupo de bovinos da região industrializada. A época de amostragem afetou a concentração dos metais Cu (soro, Zn (soro e leite, Pb (sangue e Cd (sangue e pelo, com as determinações efetuadas no verão proporcionando maiores teores do que as executadas no inverno, à exceção do Cd avaliado no pelo. Interações significativas (PThe aim of this research was to determine the heavy metals concentration in blood (Pb, Ni and Cd, serum (Cu and Zn, hair and milk (Pb, Ni, Cd, Cu and Zn of cattle raised in industrial (with steel mill and non-industrial areas in Minas Gerais, Brazil. The samples were collected during summer and winter, aiming to verify animals contamination related to environment and year season. The environment significantly influenced the concentration of Cu obtained on serum samples, with higher values for cattle from the industrialized area. The sampling time affected the concentration of Cu (serum, Zn (serum and milk, Pb (blood and Cd (blood and hair, with higher values for summer, except for Cd measured on hair. Meaningful interactions (P<0.05 between environment and year season were identified for Cu (hair and milk, Zn (hair and Ni (serum, hair and milk. The results obtained show that the presence of steel mills in a determined area does not mean, necessarily that higher concentration of heavy metals will be found in cattle biological matrices. The seasonality

  20. Data mining and biological sample exportation from South Africa: A new wave of bioexploitation under the guise of clinical care?

    Science.gov (United States)

    Staunton, Ciara; Moodley, Keymanthri

    2016-01-07

    Discovery Health, one of the leading healthcare funders in South Africa (SA), will offer genetic testing to its members for USD250 (approximately ZAR3 400) per test from 2016. On the surface, this appears to be innovative and futuristic. However, a deeper look at this announcement reveals considerable problems in the exportation of biological samples and data out of SA, and brings into sharp focus the lack of protection in place for potential donors. In return for a reduced-cost genetic test, which will nevertheless be billed to a member's savings plan, data from the patient's results, and probably the sample itself, will be sent to the USA for storage, research purposes and possible commercial use, with no further benefit for the patient. This development has demonstrated the need for more stringent protection of the movement of biological samples and data out of SA, particularly with reference to consenting procedures, material transfer agreements, and the export of biological data themselves.

  1. Determination of drugs in biological fluids by high-performance liquid chromatography with on-line sample processing.

    Science.gov (United States)

    Oertel, R; Richter, K; Gramatté, T; Kirch, W

    1998-02-27

    An automated two column HPLC system with the new packing material LiChrospher RP-18 ADS (alkyl-diol-silica) was tested for the determination of several drugs and metabolites (talinolol, celiprolol, metoprolol, oxprenolol, triamterene, trimethoprim, tiracizine, articaine, detajmium, ajmaline, lamotrigine) in various biological fluids (serum, urine, intestinal aspirates, supernatants of cell cultures and supernatants after protein denaturation). The method allows the direct injection of biological fluids into a reversed-phase HPLC system and on-line clean-up and sample enrichment by a column-switching technique. Precision, accuracy and sensitivity were similar to conventional assays as described in the literature. With this new method it was possible to measure drug concentrations in various biological fluids without changing the sample preparation procedure. In some cases an additional sample preparation like protein denaturation or solid-phase extraction was advantageous to enhance the sensitivity of the method and the life-time of the ADS column.

  2. Analysis of Investigational Drugs in Biological Fluids - Method Development and Analysis of Pre-Clinical Samples

    National Research Council Canada - National Science Library

    Lin, Emil

    2001-01-01

    ... (and metabolites and artesunate). Work on routine analyses of biological specimens during this period was performed for studies that required determination of concentrations of artelinic acid, choroquine...

  3. Characterisation of radiation field for irradiation of biological samples at nuclear reactor-comparison of twin detector and recombination methods.

    Science.gov (United States)

    Golnik, N; Gryziński, M A; Kowalska, M; Meronka, K; Tulik, P

    2014-10-01

    Central Laboratory for Radiological Protection is involved in achieving scientific project on biological dosimetry. The project includes irradiation of blood samples in radiation fields of nuclear reactor. A simple facility for irradiation of biological samples has been prepared at horizontal channel of the nuclear reactor MARIA in NCBJ in Poland. The radiation field, composed mainly of gamma radiation and thermal neutrons, has been characterised in terms of tissue kerma using twin-detector technique and recombination chambers. © The Author 2013. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  4. Accelerator mass spectrometry analysis of 14C-oxaliplatin concentrations in biological samples and 14C contents in biological samples and antineoplastic agents

    Science.gov (United States)

    Toyoguchi, Teiko; Kobayashi, Takeshi; Konno, Noboru; Shiraishi, Tadashi; Kato, Kazuhiro; Tokanai, Fuyuki

    2015-10-01

    Accelerator mass spectrometry (AMS) is expected to play an important role in microdose trials. In this study, we measured the 14C concentration in 14C-oxaliplatin-spiked serum, urine and supernatant of fecal homogenate samples in our Yamagata University (YU) - AMS system. The calibration curves of 14C concentration in serum, urine and supernatant of fecal homogenate were linear (the correlation coefficients were ⩾0.9893), and the precision and accuracy was within the acceptance criteria. To examine a 14C content of water in three vacuum blood collection tubes and a syringe were measured. 14C was not detected from water in these devices. The mean 14C content in urine samples of 6 healthy Japanese volunteers was 0.144 dpm/mL, and the intra-day fluctuation of 14C content in urine from a volunteer was little. The antineoplastic agents are administered to the patients in combination. Then, 14C contents of the antineoplastic agents were quantitated. 14C contents were different among 10 antineoplastic agents; 14C contents of paclitaxel injection and docetaxel hydrate injection were higher than those of the other injections. These results indicate that our quantitation method using YU-AMS system is suited for microdosing studies and that measurement of baseline and co-administered drugs might be necessary for the studies in low concentrations.

  5. Accelerator mass spectrometry analysis of {sup 14}C-oxaliplatin concentrations in biological samples and {sup 14}C contents in biological samples and antineoplastic agents

    Energy Technology Data Exchange (ETDEWEB)

    Toyoguchi, Teiko, E-mail: tteiko@med.id.yamagata-u.ac.jp [Department of Pharmacy, Yamagata University Hospital, 2-2-2 Iida-Nishi, Yamagata-shi, Yamagata 990-9585 (Japan); Kobayashi, Takeshi; Konno, Noboru; Shiraishi, Tadashi [Department of Pharmacy, Yamagata University Hospital, 2-2-2 Iida-Nishi, Yamagata-shi, Yamagata 990-9585 (Japan); Kato, Kazuhiro; Tokanai, Fuyuki [Department of Physics, Faculty of Science, Yamagata University, 1-4-12 Kojirakawa-machi, Yamagata-shi, Yamagata 990-8560 (Japan)

    2015-10-15

    Accelerator mass spectrometry (AMS) is expected to play an important role in microdose trials. In this study, we measured the {sup 14}C concentration in {sup 14}C-oxaliplatin-spiked serum, urine and supernatant of fecal homogenate samples in our Yamagata University (YU) – AMS system. The calibration curves of {sup 14}C concentration in serum, urine and supernatant of fecal homogenate were linear (the correlation coefficients were ⩾0.9893), and the precision and accuracy was within the acceptance criteria. To examine a {sup 14}C content of water in three vacuum blood collection tubes and a syringe were measured. {sup 14}C was not detected from water in these devices. The mean {sup 14}C content in urine samples of 6 healthy Japanese volunteers was 0.144 dpm/mL, and the intra-day fluctuation of {sup 14}C content in urine from a volunteer was little. The antineoplastic agents are administered to the patients in combination. Then, {sup 14}C contents of the antineoplastic agents were quantitated. {sup 14}C contents were different among 10 antineoplastic agents; {sup 14}C contents of paclitaxel injection and docetaxel hydrate injection were higher than those of the other injections. These results indicate that our quantitation method using YU-AMS system is suited for microdosing studies and that measurement of baseline and co-administered drugs might be necessary for the studies in low concentrations.

  6. Elemental analysis of samples of biological origin relative to their protein content by means of charged particle bombardment

    International Nuclear Information System (INIS)

    Szoekefalvi-Nagy, Z.; Demeter, I.; Varga, L.; Hollos-Nagy, K.; Keszthelyi, L.

    1981-04-01

    The particle excited X-ray emission (PIXE) and the 14 N(d,p) 15 N nuclear reaction is combined for simultaneous elemental composition and nitrogen content determination in biological samples. Using the correlation between nitrogen and proton content the elemental composition is related to the protein content of the sample. The principles and main characteristics of the method are described and illustrative applications are also given. (author)

  7. Development of a biaxial compression device for biological samples: preliminary experimental results for a closed cell foam.

    Science.gov (United States)

    Little, J P; Tevelen, G; Adam, C J; Evans, J H; Pearcy, M J

    2009-07-01

    Biological tissues are subjected to complex loading states in vivo and in order to define constitutive equations that effectively simulate their mechanical behaviour under these loads, it is necessary to obtain data on the tissue's response to multiaxial loading. Single axis and shear testing of biological tissues is often carried out, but biaxial testing is less common. We sought to design and commission a biaxial compression testing device, capable of obtaining repeatable data for biological samples. The apparatus comprised a sealed stainless steel pressure vessel specifically designed such that a state of hydrostatic compression could be created on the test specimen while simultaneously unloading the sample along one axis with an equilibrating tensile pressure. Thus a state of equibiaxial compression was created perpendicular to the long axis of a rectangular sample. For the purpose of calibration and commissioning of the vessel, rectangular samples of closed cell ethylene vinyl acetate (EVA) foam were tested. Each sample was subjected to repeated loading, and nine separate biaxial experiments were carried out to a maximum pressure of 204 kPa (30 psi), with a relaxation time of two hours between them. Calibration testing demonstrated the force applied to the samples had a maximum error of 0.026 N (0.423% of maximum applied force). Under repeated loading, the foam sample demonstrated lower stiffness during the first load cycle. Following this cycle, an increased stiffness, repeatable response was observed with successive loading. While the experimental protocol was developed for EVA foam, preliminary results on this material suggest that this device may be capable of providing test data for biological tissue samples. The load response of the foam was characteristic of closed cell foams, with consolidation during the early loading cycles, then a repeatable load-displacement response upon repeated loading. The repeatability of the test results demonstrated the

  8. The mass transfer dynamics of hollow fiber liquid-phase microextraction and its application for rapid analysis of biological samples.

    Science.gov (United States)

    Cui, Shufen; Ouyang, Gangfeng; Duan, Guijiao; Hou, Jinxing; Luan, Tiangang; Zhang, Xu

    2012-11-30

    Hollow fiber liquid-phase microextraction (HF-LPME) has been demonstrated to potentially become a mainstream sample preparation technique for complex samples. Nevertheless, the need for a relatively long extraction time is considered to be the major disadvantage of this method. Lengthy extractions may cause the loss of the extraction phase and may change the contents of biological samples via the action of enzymes. Therefore, control calibrations for particular biological systems must be made. In this study, a theoretical model of the mass transfer dynamics of two-phase HF-LPME was proposed, and the kinetic calibration (KC) of this method for plasma and urine samples was validated. The theoretical results were validated by examining the kinetics of the extraction and back-extraction processes of HF-LPME. The KC-HF-LPME method was successfully used to correct for matrix effects in plasma and urine samples during flunitrazepam analysis. The free amount of flunitrazepam was extracted from plasma for 10 min and analyzed by gas chromatography/mass spectrometry. The amount of pre-added standard and the standard remaining in the extraction phase after extraction were used for the quantification of flunitrazepam in plasma and urine samples. The new method not only significantly shortens the extraction time but also provides a new opportunity to determine the free concentration of analyte in biological systems. Copyright © 2012 Elsevier B.V. All rights reserved.

  9. Determination of D- and L-Amino Acids in Biological Samples by Two Dimensional Column Liquid Chromatography.

    NARCIS (Netherlands)

    van de Merbel, N.C.; Lingeman, H.; Brinkman, U.A.T.; Stenberg, M.; Oste, R.; Marko-Varga, G.; Gorton, L.

    1995-01-01

    A two-dimensional, column liquid chromatographic system is used for the determination of the D- and L-enantiomers of amino acids in biological samples. Separation of the amino acids is first on ion-exchange column by gradient elution with a sodium citrate-sodium chloride buffer. Enantioseparation is

  10. Development of a radiochemical neutron activation analysis procedure for determination of rhenium in biological and environmental samples at ultratrace level

    Czech Academy of Sciences Publication Activity Database

    Kučera, Jan; Byrne, A. R.; Mizera, Jiří; Lučaníková, M.; Řanda, Zdeněk

    2006-01-01

    Roč. 269, č. 2 (2006), s. 251-257 ISSN 0236-5731 R&D Projects: GA ČR(CZ) GA203/04/0943 Institutional research plan: CEZ:AV0Z10480505 Keywords : radiochemical neutron activation analysis * rhenium * biological and environmental samples Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 0.509, year: 2006

  11. 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

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

    Science.gov (United States)

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

    2016-01-28

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

  13. Estimation of calcium, magnesium, cadmium, and lead in biological samples from paralyzed quality control and production steel mill workers.

    Science.gov (United States)

    Afridi, Hassan Imran; Talpur, Farah Naz; Kazi, Tasneem Gul; Kazi, Naveed; Arain, Sadaf Sadia; Shah, Faheem

    2015-06-01

    The determination of trace and toxic metals in the biological samples of human beings is an important clinical screening procedure. The aim of the present study was to compare the level of essential trace and toxic elements cadmium (Cd), calcium (Ca), lead (Pb), and magnesium (Mg) in biological samples (whole blood, urine, and scalp hair) of male paralyzed production (PPW) and quality control workers (PQW) of a steel mill, age ranged (35-55 years). For comparison purposes, healthy age-matched exposed referent subjects (EC), working in steel mill and control subjects (NEC), who were not working in industries and lived far away from the industrial areas, were selected as control subjects. The concentrations of electrolytes and toxic elements in biological samples were measured by atomic absorption spectrometry after microwave-assisted acid digestion. The validity and accuracy of the methodology were checked using certified reference materials. The results of this study showed that the mean values of Cd and Pb were significantly higher in scalp hair, blood, and urine samples of PPW and PQW as compared to NEC and EC (p urine samples of PPW and PQW. The results show the need for immediate improvements in workplace, ventilation, and industrial hygiene practices.

  14. Use of 65 kDa mannoprotein gene primers in Real Time PCR identification of Candida albicans in biological samples.

    Science.gov (United States)

    Arancia, Silvia; Carattoli, Alessandra; La Valle, Roberto; Cassone, Antonio; De Bernardis, Flavia

    2006-10-01

    A method for the detection and quantification of Candida albicans in biological samples (blood, urine and serum) was developed with the use of Real-Time PCR utilizing CaMP65-specific primers. Two different systems were used for the detection in the LightCycler platform (Roche): the SYBR green fluorescent dye with melting peak analysis and the 5'nuclease fluorescent-probe detection. The amplification was highly specific for C. albicans, providing no cross-reaction on genomic DNA extracted from other Candida species or Aspergillus. The sensitivity in simulated biological samples was especially high (1 genome) when applied to sera and urine, and in blood samples the limit of detection was higher by ten-fold. Finally, the real-time PCR was employed in order to detect and quantify C. albicans in the sera from patients with invasive candidiasis.

  15. Microwave-ultrasound combined reactor suitable for atmospheric sample preparation procedure of biological and chemical products

    NARCIS (Netherlands)

    Lagha, A.; Chemat, S.; Bartels, P.V.; Chemat, F.

    1999-01-01

    A compact apparatus in which a specific position can be irradiated by microwaves (MW) and ultrasound (US) simultaneously has been developed. The MW-US reactor has been designed for atmospheric pressure digestion and dissolution of biological and chemical products. The reactor can treat a range of

  16. Active Learning "Not" Associated with Student Learning in a Random Sample of College Biology Courses

    Science.gov (United States)

    Andrews, T. M.; Leonard, M. J.; Colgrove, C. A.; Kalinowski, S. T.

    2011-01-01

    Previous research has suggested that adding active learning to traditional college science lectures substantially improves student learning. However, this research predominantly studied courses taught by science education researchers, who are likely to have exceptional teaching expertise. The present study investigated introductory biology courses…

  17. Biology

    Indian Academy of Sciences (India)

    I am particularly happy that the Academy is bringing out this document by Professor M S. Valiathan on Ayurvedic Biology. It is an effort to place before the scientific community, especially that of India, the unique scientific opportunities that arise out of viewing Ayurveda from the perspective of contemporary science, its tools ...

  18. Constant-Distance Mode Nanospray Desorption Electrospray Ionization Mass Spectrometry Imaging of Biological Samples with Complex Topography

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen, Son N.; Liyu, Andrey V.; Chu, Rosalie K.; Anderton, Christopher R.; Laskin, Julia

    2017-01-17

    A new approach for constant distance mode mass spectrometry imaging of biological samples using nanospray desorption electrospray ionization (nano-DESI MSI) was developed by integrating a shear-force probe with nano-DESI probe. The technical concept and basic instrumental setup as well as general operation of the system are described. Mechanical dampening of resonant oscillations due to the presence of shear forces between the probe and the sample surface enables constant-distance imaging mode via a computer controlled closed feedback loop. The capability of simultaneous chemical and topographic imaging of complex biological samples is demonstrated using living Bacillus Subtilis ATCC 49760 colonies on agar plates. The constant-distance mode nano-DESI MSI enabled imaging of many metabolites including non-ribosomal peptides (surfactin, plipastatin and iturin) and iron-bound heme on the surface of living bacterial colonies ranging in diameter from 10 mm to 13 mm with height variations of up to 0.8 mm above the agar plate. Co-registration of ion images to topographic images provided higher-contrast images. Constant-mode nano-DESI MSI is ideally suited for imaging biological samples of complex topography in their native state.

  19. Restricted access materials and large particle supports for on-line sample preparation: an attractive approach for biological fluids analysis.

    Science.gov (United States)

    Souverain, S; Rudaz, S; Veuthey, J-L

    2004-03-05

    An analytical process generally involves four main steps: (1) sample preparation; (2) analytical separation; (3) detection; and (4) data handling. In the bioanalytical field, sample preparation is often considered as the time-limiting step. Indeed, the extraction techniques commonly used for biological matrices such as liquid-liquid extraction (LLE) and solid-phase extraction (SPE) are achieved in the off-line mode. In order to perform a high throughput analysis, efforts have been engaged in developing a faster sample purification process. Among different strategies, the introduction of special extraction sorbents, such as the restricted access media (RAM) and large particle supports (LPS), allowing the direct and repetitive injection of complex biological matrices, represents a very attractive approach. Integrated in a liquid chromatography (LC) system, these extraction supports lead to the automation, simplification and speeding up of the sample preparation process. In this paper, RAM and LPS are reviewed and particular attention is given to commercially available supports. Applications of these extraction supports, are presented in single column and column-switching configurations, for the direct analysis of compounds in various biological fluids.

  20. Sampling

    CERN Document Server

    Thompson, Steven K

    2012-01-01

    Praise for the Second Edition "This book has never had a competitor. It is the only book that takes a broad approach to sampling . . . any good personal statistics library should include a copy of this book." —Technometrics "Well-written . . . an excellent book on an important subject. Highly recommended." —Choice "An ideal reference for scientific researchers and other professionals who use sampling." —Zentralblatt Math Features new developments in the field combined with all aspects of obtaining, interpreting, and using sample data Sampling provides an up-to-date treat

  1. Application of XRF and AAS for the elemental analysis of biological samples as monitors to occupational exposure

    International Nuclear Information System (INIS)

    Abdelrahman, Wafa Salih

    1999-12-01

    In the present study, hair and urine samples were collected from selected group of workers in industrial areas, and control group was collected from individuals resident far from contaminated areas. Air samples were collected form indoors atmosphere of these industries. Sudan Mint Company and Mirghani workshop are selected as a possible contaminated cities in Khartoum and Omdurman cities. X-ray fluorescence and atomic absorption techniques were applied to the analysis of the biological and air samples. AXIL computer program was used for fitting the collected spectra. The concentration of calcium, chromium, iron, cobalt, nickel, copper, zinc, bromine, and lead were evaluated. The result revealed that zinc and copper showed highest concentration in hair and air samples, while zinc was not detected in urine. In Mirghani workshop calcium, chromium, iron and zinc shows the highest values in air and hair samples also, zinc was not detected in urine. The correlation between the elemental content of the biological and environmental samples confirm that these elements can reach to the human body.(Author)

  2. Study of phosphors determination in biological samples; Estudo da determinacao de fosforo em amostras biologicas

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Rosangela Magda de

    1994-12-31

    In this paper, phosphors determination by neutron activation analysis in milk and bone samples was studied employing both instrumental and radiochemical separation methods. The analysis with radiochemistry separation consisted of the simultaneous irradiation of the samples and standards during 30 minutes, dissolution of the samples, hold back carrier, addition precipitation of phosphorus with ammonium phosphomolibdate (A.M.P.) and phosphorus-32 by counting by using Geiger-Mueller detector. The instrumental analysis consisted of the simultaneous irradiation of the samples and standards during 30 minutes, transfer of the samples into a counting planchet and measurement of the beta radiation emitted by phosphorus-32, after a suitable decay period. After the phosphorus analysis methods were established they were applied to both commercial milk and animal bone samples, and data obtained in the instrumental and radiochemical separation methods for each sample, were compared between themselves. In this work, it became possible to obtain analysis methods for phosphorus that can be applied independently of the sample quantity available, and the phosphorus content in the samples or interference that can be present in them. (author). 51 refs., 7 figs., 4 tabs.

  3. A review of the known biological characteristics of the Great Meteor East site together with a sampling programme for a biological site assessment

    International Nuclear Information System (INIS)

    Roe, H.S.J.

    1985-01-01

    Existing biological information on GME is reviewed. In common with most other oceanic areas there is very little data available from depths below 2000m. There is virtually no direct benthic information and none at all on the midwater/benthic boundary layer. Existing data from a wider geographic area are relevant to GME but the applicability of such data varies according to the hydrography. A sampling programme is outlined which will allow a comprehensive quantitative and qualitative assessment of the midwater and benthic ecosystems. Particular attention will be paid to the interactions between benthic and midwater communities just above the sea floor. (author)

  4. Testing biological liquid samples using modified m-line spectroscopy method

    Science.gov (United States)

    Augusciuk, Elzbieta; Rybiński, Grzegorz

    2005-09-01

    Non-chemical method of detection of sugar concentration in biological (animal and plant source) liquids has been investigated. Simplified set was build to show the easy way of carrying out the survey and to make easy to gather multiple measurements for error detecting and statistics. Method is suggested as easy and cheap alternative for chemical methods of measuring sugar concentration, but needing a lot effort to be made precise.

  5. Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

    OpenAIRE

    Corina Mahu Ştefania; Monica Hăncianu; Luminiţa Agoroaei; Anda Cristina Coman Băbuşanu; Elena Butnaru

    2015-01-01

    Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. ...

  6. Active Learning Not Associated with Student Learning in a Random Sample of College Biology Courses

    Science.gov (United States)

    Andrews, T. M.; Leonard, M. J.; Colgrove, C. A.; Kalinowski, S. T.

    2011-01-01

    Previous research has suggested that adding active learning to traditional college science lectures substantially improves student learning. However, this research predominantly studied courses taught by science education researchers, who are likely to have exceptional teaching expertise. The present study investigated introductory biology courses randomly selected from a list of prominent colleges and universities to include instructors representing a broader population. We examined the relationship between active learning and student learning in the subject area of natural selection. We found no association between student learning gains and the use of active-learning instruction. Although active learning has the potential to substantially improve student learning, this research suggests that active learning, as used by typical college biology instructors, is not associated with greater learning gains. We contend that most instructors lack the rich and nuanced understanding of teaching and learning that science education researchers have developed. Therefore, active learning as designed and implemented by typical college biology instructors may superficially resemble active learning used by education researchers, but lacks the constructivist elements necessary for improving learning. PMID:22135373

  7. Active learning not associated with student learning in a random sample of college biology courses.

    Science.gov (United States)

    Andrews, T M; Leonard, M J; Colgrove, C A; Kalinowski, S T

    2011-01-01

    Previous research has suggested that adding active learning to traditional college science lectures substantially improves student learning. However, this research predominantly studied courses taught by science education researchers, who are likely to have exceptional teaching expertise. The present study investigated introductory biology courses randomly selected from a list of prominent colleges and universities to include instructors representing a broader population. We examined the relationship between active learning and student learning in the subject area of natural selection. We found no association between student learning gains and the use of active-learning instruction. Although active learning has the potential to substantially improve student learning, this research suggests that active learning, as used by typical college biology instructors, is not associated with greater learning gains. We contend that most instructors lack the rich and nuanced understanding of teaching and learning that science education researchers have developed. Therefore, active learning as designed and implemented by typical college biology instructors may superficially resemble active learning used by education researchers, but lacks the constructivist elements necessary for improving learning.

  8. Fast screening of glycosaminoglycan disaccharides by fluorophore-assisted carbohydrate electrophoresis (FACE): applications to biologic samples and pharmaceutical formulations.

    Science.gov (United States)

    Karousou, Evgenia; Asimakopoulou, Athanasia P; Zafeiropoulou, Vassiliki; Viola, Manuela; Monti, Luca; Rossi, Antonio; Passi, Alberto; Karamanos, Nikos

    2015-01-01

    Hyaluronan (HA), chondroitin sulfate (CS), and heparan sulfate (HS) are glycosaminoglycans (GAGs) with a great importance in biological processes as they participate in functional cell properties, such as migration, adhesion, and proliferation. A perturbation of the quantity and/or the sulfation of GAGs is often associated with pathological conditions. In this chapter, we present valuable and validated protocols for the analysis of HA-, CS-, and HS-derived disaccharides after derivatization with 2-aminoacridone and by using the fluorophore-assisted carbohydrate electrophoresis (FACE). FACE is a well-known technique and a reliable tool for a fast screening of GAGs, as it is possible to analyze 16 samples at the same time with one electrophoretic apparatus. The protocols for the gel preparation are based on the variations of the acrylamide/bisacrylamide and buffer concentrations. Different approaches for the extraction and purification of the disaccharides of various biologic samples and pharmaceutical preparations are also stressed.

  9. Study of the relationship between peaks scattering Rayleigh to Compton ratio and effective atomic number in biological samples

    International Nuclear Information System (INIS)

    Pereira, Marcelo O.; Conti, Claudio de Carvalho; Anjos, Marcelino J.; Lopes, Ricardo T.

    2011-01-01

    The aim of this work was to develop a new method to correct the absorbed radiation (the mass attenuation coefficient curve) in low energy (E B O 3 , Na 2 CO 3 , CaCO 3 , Al 2 O 3 , K 2 SO 4 and MgO) of radiation produced by a gamma-ray source of Am-241(59.54 keV) also applied to certified biological samples of milk powder, hay powder and bovine liver (NIST 155 7B). In addition, six methods of effective atomic number determination were used as described in literature to determinate the Rayleigh to Compton scattering ratio (R/C) , in order to calculate the mass attenuation coefficient. The results obtained by the proposed method were compared with those obtained using the transmission method. The experimental results were in good agreement with transmission values suggesting that the method to correct radiation absorption presented in this paper is adequate for biological samples. (author)

  10. Gelatin embedding: a novel way to preserve biological samples for terahertz imaging and spectroscopy

    International Nuclear Information System (INIS)

    Fan, Shuting; Ung, Benjamin; Parrott, Edward P J; Pickwell-MacPherson, Emma

    2015-01-01

    Sample dehydration has traditionally been a challenging problem in ex vivo terahertz biomedical experiments as water content changes significantly affect the terahertz properties and can diminish important contrast features. In this paper, we propose a novel method to prevent sample dehydration using gelatin embedding. By looking at terahertz image data and calculating the optical properties of the gelatin-embedded sample, we find that our method successfully preserves the sample for at least 35 h, both for imaging and spectroscopy. Our novel preservation method demonstrates for the first time the capability to simultaneously maintain sample structural integrity and prevent dehydration at room temperature. This is particularly relevant for terahertz studies of freshly excised tissues but could be beneficial for other imaging and spectroscopy techniques. (paper)

  11. Preparing monodisperse macromolecular samples for successful biological small-angle X-ray and neutron-scattering experiments.

    Science.gov (United States)

    Jeffries, Cy M; Graewert, Melissa A; Blanchet, Clément E; Langley, David B; Whitten, Andrew E; Svergun, Dmitri I

    2016-11-01

    Small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume, including the solvent and buffer components, as well as the macromolecules of interest. To obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis, so it is essential that the samples be pure and monodisperse for the duration of the experiment. This protocol outlines the basic physics of SAXS and SANS, and it reveals how the underlying conceptual principles of the techniques ultimately 'translate' into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size-exclusion chromatography (SEC) and light scattering. Also included are procedures that are specific to X-rays (in-line SEC-SAXS) and neutrons, specifically preparing samples for contrast matching or variation experiments and deuterium labeling of proteins.

  12. Preparing Monodisperse Macromolecular Samples for Successful Biological Small-Angle X-ray and Neutron Scattering Experiments

    Science.gov (United States)

    Jeffries, Cy M.; Graewert, Melissa A.; Blanchet, Clément E.; Langley, David B.; Whitten, Andrew E.; Svergun, Dmitri I

    2017-01-01

    Small-angle X-ray and neutron scattering (SAXS and SANS) are techniques used to extract structural parameters and determine the overall structures and shapes of biological macromolecules, complexes and assemblies in solution. The scattering intensities measured from a sample contain contributions from all atoms within the illuminated sample volume including the solvent and buffer components as well as the macromolecules of interest. In order to obtain structural information, it is essential to prepare an exactly matched solvent blank so that background scattering contributions can be accurately subtracted from the sample scattering to obtain the net scattering from the macromolecules in the sample. In addition, sample heterogeneity caused by contaminants, aggregates, mismatched solvents, radiation damage or other factors can severely influence and complicate data analysis so it is essential that the samples are pure and monodisperse for the duration of the experiment. This Protocol outlines the basic physics of SAXS and SANS and reveals how the underlying conceptual principles of the techniques ultimately ‘translate’ into practical laboratory guidance for the production of samples of sufficiently high quality for scattering experiments. The procedure describes how to prepare and characterize protein and nucleic acid samples for both SAXS and SANS using gel electrophoresis, size exclusion chromatography and light scattering. Also included are procedures specific to X-rays (in-line size exclusion chromatography SAXS) and neutrons, specifically preparing samples for contrast matching/variation experiments and deuterium labeling of proteins. PMID:27711050

  13. Analysis of Investigational Drugs in Biological Fluids- Method Development and Analysis of Pre-Clinical and Clinical Samples.

    Science.gov (United States)

    1999-09-01

    to reach equilibrium with erythrocytes. Sample Preparation Procedures Suitable preparation of the biological specimens is essential for the...antibiotics that are zwitterionic in nature, generally possess very low water-to- oil partition coefficients and, thus, are extremely difficult to...antileishmanial drug in hamsters infected with Leishmania donovani .9 Because antimony compounds are not always effective and the other drugs in use have

  14. Cathepsin D : design and characterisation of new in vitro and in vivo substrates applied to biological samples

    OpenAIRE

    Bächle, Daniel

    2005-01-01

    The specific and sensitive detection of protease activities within aqueous biological fluids such as blood, urine, sweat or cell lysates is important since proteases are widely used biomarkers for the discrimination between diseased and healthy samples. Recently, great efforts have been made to develop new proteomic approaches implying screening studies for the parallel determination of various parameters. Therefore specific and high-throughput compatible methods are required. The present wor...

  15. Fluorometric quantification of protoporphyrin IX in biological skin samples from in vitro penetration/permeation studies

    Directory of Open Access Journals (Sweden)

    Fábia Cristina Rossetti

    2010-12-01

    Full Text Available A fluorometric analytical method was developed for quantification of protoporphyrin IX (PpIX in skin samples and receptor phase solution after in vitro cutaneous penetration/permeation studies. Analytical conditions used were: excitation and emission wavelengths: 400 nm and 632 nm; bandwidth: 0.5 nm; excitation and emission slits: 10/10. PpIX was recovered from two different layers of skin, the stratum corneum (SC and the epidermis plus dermis ([E+D], by vortex homogenization, probe and bath sonication, using DMSO as an extraction solvent. The detection and quantification limits were 0.002 and 0.005 μg/mL, respectively. The assay was linear from 0.005 - 0.5 μg/mL. The within-day and between-day assay precision and accuracy in DMSO and receptor phase solution were each studied at the two concentration levels 0.04 and 0.2 μg/mL, and 0.01 and 0.08 μg/mL, respectively. The coefficients of variation and deviation from the theoretical values were lower than 5%. The skin recovery of PpIX from SC and [E+D] layers using two different concentrations (0.5 and 1.0 μg/mL were all above 90.0%. The method described has potential application to in vitro penetration/permeation studies of PpIX using porcine skin as a biological membrane model.Um método analítico por espectrofluorimetria foi desenvolvido para quantificar a protoporfirina IX (Pp IX em amostras de pele e fase receptora após a realização de testes in vitro de penetração/permeação cutâneas. As condições analíticas utilizadas foram: comprimentos de onda de excitação e emissão: 400 nm e 632 nm; largura de banda: 0,5 nm; fendas de excitação e emissão: 10/10. A PpIX foi extraída de amostras de estrato córneo (EC e da epiderme sem estrato córneo + derme ([E+D] através da agitação em vórtex e sonicação por haste e banho, utilizando-se o DMSO como solvente extrator. O limite de detecção e quantificação foram, respectivamente, de 0,002 e 0,005 μg/mL. O método mostrou

  16. Optimized IMAC-IMAC protocol for phosphopeptide recovery from complex biological samples

    DEFF Research Database (Denmark)

    Ye, Juanying; Zhang, Xumin; Young, Clifford

    2010-01-01

    using Fe(III)-NTA IMAC resin and it proved to be highly selective in the phosphopeptide enrichment of a highly diluted standard sample (1:1000) prior to MALDI MS analysis. We also observed that a higher iron purity led to an increased IMAC enrichment efficiency. The optimized method was then adapted...... to phosphoproteome analyses of cell lysates of high protein complexity. From either 20 microg of mouse sample or 50 microg of Drosophila melanogaster sample, more than 1000 phosphorylation sites were identified in each study using IMAC-IMAC and LC-MS/MS. We demonstrate efficient separation of multiply phosphorylated...... characterization of phosphoproteins in functional phosphoproteomics research projects....

  17. Use of fast atom bombardment mass spectrometry (FAB MS) for the analysis of zinc stable isotopes in biological samples

    International Nuclear Information System (INIS)

    Peirce, P.; Fennessey, P.; Hambidge, M.; Miller, L.; Goss, C.

    1986-01-01

    The use of stable isotopes offer a means of measuring human metabolism of trace metals in populations in which radioisotopes are contraindicated. The objective of this research has been to develop stable isotope methodology for the measurement of zinc in biological samples and to apply this methodology in pilot studies of intestinal zinc absorption. Analyses were made with a VG 7070E HF sector mass spectrometer at a resolution of 3000. Samples of 10 μl containing approximately 1 μg Zn were applied directly to a gold target, dried and inserted into the FAB source for ionization. Precision at the 1% level of enrichment was 2% (RSD). Pilot studies of the clinical application have been undertaken on two subjects to each of whom a single oral dose of enriched 70 Zn was administered after an overnight fast. A comparison of aqueous standards and prepared fecal samples showed undetectable levels of contamination at the 64 Zn to 70 Zn masses. Precision of fecal samples is comparable to that of aqueous standards. Calculated absorption after an overnight fast was between 60-65% of the administered dose. The FAB MS provides a simple, sensitive and precise technique for the measurement of zinc stable isotopes in biological samples

  18. Automatic sampling for unbiased and efficient stereological estimation using the proportionator in biological studies

    DEFF Research Database (Denmark)

    Gardi, Jonathan Eyal; Nyengaard, Jens Randel; Gundersen, Hans Jørgen Gottlieb

    2008-01-01

    Quantification of tissue properties is improved using the general proportionator sampling and estimation procedure: automatic image analysis and non-uniform sampling with probability proportional to size (PPS). The complete region of interest is partitioned into fields of view, and every field...... of view is given a weight (the size) proportional to the total amount of requested image analysis features in it. The fields of view sampled with known probabilities proportional to individual weight are the only ones seen by the observer who provides the correct count. Even though the image analysis...... cerebellum, total number of orexin positive neurons in transgenic mice brain, and estimating the absolute area and the areal fraction of β islet cells in dog pancreas.  The proportionator was at least eight times more efficient (precision and time combined) than traditional computer controlled sampling....

  19. Study of performance characteristics of a radiochemical method to determine uranium in biological samples

    International Nuclear Information System (INIS)

    Puga, Maria J.; Cerchietti, Maria L.R.; Prudenzo, J.E.; Arguelles, Maria G.

    2005-01-01

    In this paper is described a methodology to calculate detection limit (Ld), quantification level (Lq) and minimum detectable activity (MDA) in a radiochemical method for determination of uranium in urine samples. The concentration is measured by fluorimetry and alpha gross activity using liquid scintillation counting (LSC). The calculation of total propagated uncertainty on a spike sample is presented. Furthermore, the major sources of uncertainty and percentage contribution in both measurements are assessed. (author)

  20. Sample Preparation for Determination of Biological Thiols by Liquid Chromatography and Electromigration Techniques

    OpenAIRE

    Bald, Edward

    2004-01-01

    Wydrukowano z dostarczonych Wydawnictwu UŁ gotowych materiałów Majority of the bioanalytical or environmental methods do not use just one chromatografie or electrophoretic step, but rather involve several sample pretreatment steps which simplfy the matrix, and often preconcentrate and chemically modify the analytes. This work surveys typical procedures for sample preparation for most commonly analyzed biofluids with particular emphasis placed on chemical derivatization of su...

  1. The scope of detector Medipix2 in micro-radiography of biological samples

    Czech Academy of Sciences Publication Activity Database

    Dammer, J.; Weyda, František; Jakůbek, J.; Škrabal, P.; Sopko, V.; Vavřík, D.

    2011-01-01

    Roč. 633, č. 1 (2011), s. 175-176 ISSN 0168-9002. [International Workshop on Radiation Imaging Detectors /11./. Praha, 29.06.2009-03.07.2009] R&D Projects: GA MŠk 2B06005 Grant - others:Ministerstvo školství(CZ) 6840770040; GA MŠk(CZ) 1P04LA211; GA MŠk(CZ) LC06041 Program:1P; LC Institutional research plan: CEZ:AV0Z50070508 Keywords : x-ray imaging * digital radiography * photon and x-ray detectors Subject RIV: EA - Cell Biology Impact factor: 1.207, year: 2011

  2. Development of tomographic reconstruction algorithms for the PIXE analysis of biological samples

    International Nuclear Information System (INIS)

    Nguyen, D.T.

    2008-05-01

    The development of 3-dimensional microscopy techniques offering a spatial resolution of 1 μm or less has opened a large field of investigation in Cell Biology. Amongst them, an interesting advantage of ion beam micro-tomography is its ability to give quantitative results in terms of local concentrations in a direct way, using Particle Induced X-ray Emission (PIXET) combined to Scanning Transmission Ion Microscopy (STIMT) Tomography. After a brief introduction of existing reconstruction techniques, we present the principle of the DISRA code, the most complete written so far, which is the basis of the present work. We have modified and extended the DISRA algorithm by considering the specific aspects of biologic specimens. Moreover, correction procedures were added in the code to reduce noise in the tomograms. For portability purpose, a Windows graphic interface was designed to easily enter and modify experimental parameters used in the reconstruction, and control the several steps of data reduction. Results of STIMT and PIXET experiments on reference specimens and on human cancer cells will be also presented. (author)

  3. Development of a radioimmunoassay for the determination of buprenorphine in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Debrabandere, L.; Boven, M. Van; Daenens, P. (Louvain Univ. (Belgium))

    1993-02-01

    The development of a specific and sensitive radioimmunoassay for the detection of buprenorphine in urine samples is described. With minor adjustments, the assay was also applied to the analysis for buprenorphine in plasma samples. The 2-diazobenzoic acid derivative of buprenorphine has been prepared as a hapten. The immunization of rabbits with the hapten-bovine serum albumin conjugate resulted in the production of antibodies, which cross-reacted with N-dealkylbuprenophine up to about the 90% level. The antibodies showed very low cross-reactivities with the 3-O-glucuronides and with the structural analogue etorphine. The assay was mainly used to prescreen for buprenorphine in urine samples of persons suspected of Temgesic misuse and to determine buprenorphine in plasma samples. A linear calibration graph for buprenorphine was obtained after logit-log regression. The spiking recovery study showed a linear regression. Intra-and inter-assay relative standard deviations were < 4.35 and < 6.36%, respectively. A comparison study of the high-performance liquid chromatographic determination (X) to the radioimmunoassay (Y) resulted in the following regression equation for the urine samples: Y = 1.44 + 1.64 X (n = 32; r 0.910) and Y = 0.007 + 1.58 X (n = 10; r = 0.930) for plasma specimens. The minimum detectable dose of the immunoassay was calculated to be 10 pg ml[sup -1] (Student's t-distribution, p 0.01, degrees of freedom = 8). (Author).

  4. Direct quantification of lipopeptide biosurfactants in biological samples via HPLC and UPLC-MS requires sample modification with an organic solvent.

    Science.gov (United States)

    Biniarz, Piotr; Łukaszewicz, Marcin

    2017-06-01

    The rapid and accurate quantification of biosurfactants in biological samples is challenging. In contrast to the orcinol method for rhamnolipids, no simple biochemical method is available for the rapid quantification of lipopeptides. Various liquid chromatography (LC) methods are promising tools for relatively fast and exact quantification of lipopeptides. Here, we report strategies for the quantification of the lipopeptides pseudofactin and surfactin in bacterial cultures using different high- (HPLC) and ultra-performance liquid chromatography (UPLC) systems. We tested three strategies for sample pretreatment prior to LC analysis. In direct analysis (DA), bacterial cultures were injected directly and analyzed via LC. As a modification, we diluted the samples with methanol and detected an increase in lipopeptide recovery in the presence of methanol. Therefore, we suggest this simple modification as a tool for increasing the accuracy of LC methods. We also tested freeze-drying followed by solvent extraction (FDSE) as an alternative for the analysis of "heavy" samples. In FDSE, the bacterial cultures were freeze-dried, and the resulting powder was extracted with different solvents. Then, the organic extracts were analyzed via LC. Here, we determined the influence of the extracting solvent on lipopeptide recovery. HPLC methods allowed us to quantify pseudofactin and surfactin with run times of 15 and 20 min per sample, respectively, whereas UPLC quantification was as fast as 4 and 5.5 min per sample, respectively. Our methods provide highly accurate measurements and high recovery levels for lipopeptides. At the same time, UPLC-MS provides the possibility to identify lipopeptides and their structural isoforms.

  5. Diffraction enhanced imaging and x-ray fluorescence microtomography for analyzing biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Rocha, H.S.; Pereira, G.R.; Lopes, R.T. [Laboratorio de Instrumentacao Nuclear-COPPE/UFRJ-RJ (Brazil); Anjos, M.J. [Instituto de Fisica-UERJ-RJ (Brazil); Faria, P. [Instituto Nacional do Cancer-INCa-RJ (Brazil); Kellermann, G.; Perez, C.A. [Laboratorio Nacional de Luz Sincrotron-Campinas-SP (Brazil); Tirao, G. [Faculdad de Mat. Astronomia y Fisica (FAMAF), UNC. Cordoba (Argentina); Mazzaro, I. [Laboratorio de Optica de Raios X e Instrumentacao-UFPR-Curitiba-PR (Brazil); Giles, C. [Laboratorio de Cristalografia Aplicada e Raios X-UNICAMP-Campinas-SP (Brazil)

    2007-07-15

    In this work, breast tissue samples were investigated in order to verify the distribution of certain elements by x-ray fluorescence computed tomography (XRFCT) correlated with the characteristics and pathology of each tissue observed by diffraction enhanced imaging (DEI). The DEI system can show details in low attenuation tissues. It is based on the contrast imaging obtained by extinction, diffraction and refraction characteristics and can improve reduction in false positive and false negative diagnoses. XRFCT allows mapping of all elements within the sample, since even a minute fluorescence signal can be detected. DEI imaging techniques revealed the complex structure of the disease, confirmed by the histological section, and showed microstructures in all planes of the sample. The XRFCT showed the distribution of Zn, Cu and Fe at higher concentration. (authors)

  6. A combined method for correlative 3D imaging of biological samples from macro to nano scale

    Science.gov (United States)

    Kellner, Manuela; Heidrich, Marko; Lorbeer, Raoul-Amadeus; Antonopoulos, Georgios C.; Knudsen, Lars; Wrede, Christoph; Izykowski, Nicole; Grothausmann, Roman; Jonigk, Danny; Ochs, Matthias; Ripken, Tammo; Kühnel, Mark P.; Meyer, Heiko

    2016-10-01

    Correlative analysis requires examination of a specimen from macro to nano scale as well as applicability of analytical methods ranging from morphological to molecular. Accomplishing this with one and the same sample is laborious at best, due to deformation and biodegradation during measurements or intermediary preparation steps. Furthermore, data alignment using differing imaging techniques turns out to be a complex task, which considerably complicates the interconnection of results. We present correlative imaging of the accessory rat lung lobe by combining a modified Scanning Laser Optical Tomography (SLOT) setup with a specially developed sample preparation method (CRISTAL). CRISTAL is a resin-based embedding method that optically clears the specimen while allowing sectioning and preventing degradation. We applied and correlated SLOT with Multi Photon Microscopy, histological and immunofluorescence analysis as well as Transmission Electron Microscopy, all in the same sample. Thus, combining CRISTAL with SLOT enables the correlative utilization of a vast variety of imaging techniques.

  7. Supercritical Fluid Extraction and Ultra Performance Liquid Chromatography of Respiratory Quinones for Microbial Community Analysis in Environmental and Biological Samples

    Directory of Open Access Journals (Sweden)

    Koichi Fujie

    2012-03-01

    Full Text Available Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE and ultra performance liquid chromatography (UPLC method for the analysis of bacterial respiratory quinones (RQ in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA detector was successfully applied to the simultaneous determination of ubiquinones (UQ and menaquinones (MK without tedious pretreatment. Supercritical carbon dioxide (scCO2 extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost and biological samples (swine and Japanese quail feces.

  8. Supercritical fluid extraction and ultra performance liquid chromatography of respiratory quinones for microbial community analysis in environmental and biological samples.

    Science.gov (United States)

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

    2012-03-05

    Microbial community structure plays a significant role in environmental assessment and animal health management. The development of a superior analytical strategy for the characterization of microbial community structure is an ongoing challenge. In this study, we developed an effective supercritical fluid extraction (SFE) and ultra performance liquid chromatography (UPLC) method for the analysis of bacterial respiratory quinones (RQ) in environmental and biological samples. RQ profile analysis is one of the most widely used culture-independent tools for characterizing microbial community structure. A UPLC equipped with a photo diode array (PDA) detector was successfully applied to the simultaneous determination of ubiquinones (UQ) and menaquinones (MK) without tedious pretreatment. Supercritical carbon dioxide (scCO(2)) extraction with the solid-phase cartridge trap proved to be a more effective and rapid method for extracting respiratory quinones, compared to a conventional organic solvent extraction method. This methodology leads to a successful analytical procedure that involves a significant reduction in the complexity and sample preparation time. Application of the optimized methodology to characterize microbial communities based on the RQ profile was demonstrated for a variety of environmental samples (activated sludge, digested sludge, and compost) and biological samples (swine and Japanese quail feces).

  9. Unrealistic optimism, fatalism, and risk-taking in New Zealand farmers' descriptions of quad-bike incidents: a directed qualitative content analysis.

    Science.gov (United States)

    Clay, Lynne; Hay-Smith, E Jean C; Treharne, Gareth J; Milosavljevic, Stephan

    2015-01-01

    Quad-bike incidents are a major cause of occupational injury and fatality on farms warranting health and safety attention. As part of a larger study, we carried out a face-to-face survey with 216 farmers in New Zealand. We quantitatively identified farmers' propensity for risk-taking, unrealistic optimism, and fatalism as risk factors in quad-bike loss-of-control events (LCEs). The purpose of the analysis presented in this article was to use these same farmers' recollections of LCEs to explore the a priori constructs in more detail using qualitative methods. Participants reporting one or more LCEs described their first LCE and any experienced in the previous 12 months. Participants provided open-text responses about what occurred at each LCE, their reflections, and general thoughts on LCE risk factors. Directed qualitative content analysis (QCA) was used to "unpack" risk-taking, unrealistic optimism, and fatalism whilst also delineating any additional concepts that farmers associate with LCEs. Risk-taking elements were more evident than unrealistic optimism or fatalism and more suggestive of farmers finding themselves in risky situations rather than engaging in risk-seeking behavior per se. Additional inductively derived categories of fatigue/stress, multitasking, inexperience, and quad-bike faults highlight the complex nature of LCEs and the importance of risk assessment covering these concepts as well as risky situations.

  10. Resonant Mie scattering (RMieS) correction of infrared spectra from highly scattering biological samples.

    Science.gov (United States)

    Bassan, Paul; Kohler, Achim; Martens, Harald; Lee, Joe; Byrne, Hugh J; Dumas, Paul; Gazi, Ehsan; Brown, Michael; Clarke, Noel; Gardner, Peter

    2010-02-01

    Infrared spectra of single biological cells often exhibit the 'dispersion artefact' observed as a sharp decrease in intensity on the high wavenumber side of absorption bands, in particular the Amide I band at approximately 1655 cm(-1), causing a downward shift of the true peak position. The presence of this effect makes any biochemical interpretation of the spectra unreliable. Recent theory has shed light on the origins of the 'dispersion artefact' which has been attributed to resonant Mie scattering (RMieS). In this paper a preliminary algorithm for correcting RMieS is presented and evaluated using simulated data. Results show that the 'dispersion artefact' appears to be removed; however, the correction is not perfect. An iterative approach was subsequently implemented whereby the reference spectrum is improved after each iteration, resulting in a more accurate correction. Consequently the corrected spectra become increasingly more representative of the pure absorbance spectra. Using this correction method reliable peak positions can be obtained.

  11. ANALYTICAL TECHNIQUES FOR THE DETERMINATION OF MELOXICAM IN PHARMACEUTICAL FORMULATIONS AND BIOLOGICAL SAMPLES

    Directory of Open Access Journals (Sweden)

    Aisha Noreen

    2016-06-01

    Full Text Available Meloxicam (MX belongs to the family of oxicams which is the most important group of non steroidal anti-inflammatory drugs (NSAIDs and is widely used for their analgesics and antipyretic activities. It inhibits both COX-I and COX-II enzymes with less gastric and local tissues irritation. A number of analytical techniques have been used for the determination of MX in pharmaceutical as well as in biological fluids. These techniques include titrimetry, spectrometry, chromatography, flow injection spectrometry, fluorescence spectrometry, capillary zone electrophoresis and electrochemical techniques. Many of these techniques have also been used for the simultaneous determination of MX with other compounds. A comprehensive review of these analytical techniques has been done which could be useful for the analytical chemists and quality control pharmacists.

  12. Multiplexed two-photon microscopy of dynamic biological samples with shaped broadband pulses.

    Science.gov (United States)

    Pillai, Rajesh S; Boudoux, Caroline; Labroille, Guillaume; Olivier, Nicolas; Veilleux, Israel; Farge, Emmanuel; Joffre, Manuel; Beaurepaire, Emmanuel

    2009-07-20

    Coherent control can be used to selectively enhance or cancel concurrent multiphoton processes, and has been suggested as a means to achieve nonlinear microscopy of multiple signals. Here we report multiplexed two-photon imaging in vivo with fast pixel rates and micrometer resolution. We control broadband laser pulses with a shaping scheme combining diffraction on an optically-addressed spatial light modulator and a scanning mirror allowing to switch between programmable shapes at kiloHertz rates. Using coherent control of the two-photon excited fluorescence, it was possible to perform selective microscopy of GFP and endogenous fluorescence in developing Drosophila embryos. This study establishes that broadband pulse shaping is a viable means for achieving multiplexed nonlinear imaging of biological tissues.

  13. Determination of some trace elements in biological samples using XRF and TXRF techniques

    International Nuclear Information System (INIS)

    Khuder, A.; Karjou, J.; Sawan, M. K.

    2006-07-01

    XRF and TXRF techniques were successfully used for the multi-element determination of trace elements in whole blood and human head hair samples. This was achieved by the direct analysis using XRF technique with different collimation units and by the optimized chemical procedures for TXRF analysis. Light element of S and P were preferably determined by XRF with primary x-ray excitation, while, elements of K, Ca, Fe, and Br were determined with a very good accuracy and precision using XRF with Cu- and Mo-secondary targets. The chemical procedure dependent on the preconcentration of trace elements by APDC was superiorly used for the determination of traces of Ni and Pb in the range of 1.0-1.7 μg/dl and 11-23 μg/dl, respectively, in whole blood samples by TXRF technique; determination of other elements as Cu and Zn was also achievable using this approach. Rb in whole blood samples was determined directly after the digestion of samples using PTFE-bomb for TXRF analysis. (author)

  14. Analysis of mercury and selenium in biological samples by neutron activation analysis

    International Nuclear Information System (INIS)

    Catharino, Marilia Gabriela Miranda

    2002-01-01

    In the present work, hair samples from populations suspected of contamination by mercury, in the localities of Serra do Navio, Vila Nova and Tartarugalzinho, in the State of Amapa, were analyzed. Hair samples of children under odontopediatric treatment were also analyzed for mercury, in order to study the possibility of transfer of mercury from the dental amalgam and also to obtain data of hair mercury in a control population of children. Another step of the work was the development of a method for the determination of selenium, by using the short-lived radioisotope 77 mSe. After the certification of the method it was applied to the analysis of hair, nails and a vitamin supplement. A comparison was made with the results obtain ed by using the long-lived radioisotope of selenium, 75 Se. The results obtained for mercury in the hair samples of populations living in the State of Amapa have shown that the mercury concentrations in these populations are much higher than in the controls. As for the hair samples of children under treatment with mercury amalgam, no significant differences were found in the concentrations of mercury after the treatment. On the other hand, these data were important to obtain data for a control population of children. The results obtained by using the radioisotope 77 mSe showed that the method developed was suitable for the analyzed matrixes and the results were similar to the ones obtained by employing the usual AANI method, with the radioisotope 75 Se. (author)

  15. Development of a radioimmunoassay for the determination of buprenorphine in biological samples

    International Nuclear Information System (INIS)

    Debrabandere, L.; Boven, M. Van; Daenens, P.

    1993-01-01

    The development of a specific and sensitive radioimmunoassay for the detection of buprenorphine in urine samples is described. With minor adjustments, the assay was also applied to the analysis for buprenorphine in plasma samples. The 2-diazobenzoic acid derivative of buprenorphine has been prepared as a hapten. The immunization of rabbits with the hapten-bovine serum albumin conjugate resulted in the production of antibodies, which cross-reacted with N-dealkylbuprenophine up to about the 90% level. The antibodies showed very low cross-reactivities with the 3-O-glucuronides and with the structural analogue etorphine. The assay was mainly used to prescreen for buprenorphine in urine samples of persons suspected of Temgesic misuse and to determine buprenorphine in plasma samples. A linear calibration graph for buprenorphine was obtained after logit-log regression. The spiking recovery study showed a linear regression. Intra-and inter-assay relative standard deviations were -1 (Student's t-distribution, p 0.01, degrees of freedom = 8). (Author)

  16. Phase microscopy of technical and biological samples through random phase modulation with a difuser

    DEFF Research Database (Denmark)

    Almoro, Percival; Pedrini, Giancarlo; Gundu, Phanindra Narayan

    2010-01-01

    A technique for phase microscopy using a phase diffuser and a reconstruction algorithm is proposed. A magnified specimen wavefront is projected on the diffuser plane that modulates the wavefront into a speckle field. The speckle patterns at axially displaced planes are sampled and used......) 2010 Optical Society of America...

  17. A retrospective cross-sectional quantitative molecular approach in biological samples from patients with syphilis.

    Science.gov (United States)

    Pinto, Miguel; Antelo, Minia; Ferreira, Rita; Azevedo, Jacinta; Santo, Irene; Borrego, Maria José; Gomes, João Paulo

    2017-03-01

    Syphilis is the sexually transmitted disease caused by Treponema pallidum, a pathogen highly adapted to the human host. As a multistage disease, syphilis presents distinct clinical manifestations that pose different implications for diagnosis. Nevertheless, the inherent factors leading to diverse disease progressions are still unknown. We aimed to assess the association between treponemal loads and dissimilar disease outcomes, to better understand syphilis. We retrospectively analyzed 309 DNA samples distinct anatomic sites associated with particular syphilis manifestations. All samples had previously tested positive by a PCR-based diagnostic kit. An absolute quantitative real-time PCR procedure was used to precisely quantify the number of treponemal and human cells to determine T. pallidum loads in each sample. In general, lesion exudates presented the highest T. pallidum loads in contrast with blood-derived samples. Within the latter, a higher dispersion of T. pallidum quantities was observed for secondary syphilis. T. pallidum was detected in substantial amounts in 37 samples of seronegative individuals and in 13 cases considered as syphilis-treated. No association was found between treponemal loads and serological results or HIV status. This study suggests a scenario where syphilis may be characterized by: i) heterogeneous and high treponemal loads in primary syphilis, regardless of the anatomic site, reflecting dissimilar duration of chancres development and resolution; ii) high dispersion of bacterial concentrations in secondary syphilis, potentially suggesting replication capability of T. pallidum while in the bloodstream; and iii) bacterial evasiveness, either to the host immune system or antibiotic treatment, while remaining hidden in privileged niches. This work highlights the importance of using molecular approaches to study uncultivable human pathogens, such as T. pallidum, in the infection process. Copyright © 2017 Elsevier Ltd. All rights

  18. Determination of sodium in biological samples by instrumental neutron activation analysis

    International Nuclear Information System (INIS)

    Parwate, D.V.; Garg, A.N.

    1981-01-01

    Sodium is one of the most essential elements needed for metabolic processes amongst human beings. It is consumed in the form of sodium chloride but it is also present in edible plant leaves. Sodium is mostly analyzed by flame photometric method, a destructive and time consuming technique. Sodium has been determined in some green leave vegetables samples-palak, radish, khatta palak (ambat chuka), chaulai leaves, chauli bean covers and its seeds by instrumental neutron activation analysis. The method involves irradiation of samples with thermal neutrons from 241 Am-Be source and counting 24 Na activity (half life 15 hr) from the reaction 23 Na(n,γ) 24 Na. Activity due to 1.37 MeV photopeak was counted with a NaI(Tl) crystal coupled to gamma ray spectrometer. Green leaves of the vegetables were thoroughly washed, dried at constant temperature and powdered. Bowen's Kale powder was used as standard for measuring sodium abundances. About 2g each of samples and the standard were packed in polythene vials. They were irradiated for 24 hrs, delayed by 1 hr and then counted for 20 mts. It is found that radish leaves are most enriched in sodium (14.0 +-0.45%) amongst four leave samples analyzed. For three different parts of chaulai leaves, bean covers and seeds, sodium contents are 1.38%, 1820 and 1010 ppm. Palak contains 2.84 +-0.29% while khatta palak contains only 4210 +- 830 ppm sodium. All values reported here are for dry weight samples and are means of three replicate measurements with standard deviation. (author)

  19. Headspace solid-phase microextraction with 1-pyrenyldiazomethane on-fibre derivatisation for analysis of fluoroacetic acid in biological samples.

    Science.gov (United States)

    Sporkert, Frank; Pragst, Fritz; Hübner, Sandra; Mills, Graham

    2002-05-25

    A new and in part automated headspace solid-phase microextraction method for quantitative determination of the highly toxic rodenticide fluoroacetic acid (FAA) in serum and other biological samples has been developed. FAA and deuterated acetic acid (internal standard) were extracted from acidified samples by a StableFlex divinylbenzene-Carboxen on polydimethylsiloxane fibre. The acids were derivatised on the fibre in-situ with 1-pyrenyldiazomethane and detected using gas chromatography-mass spectrometry with electron impact ionisation and selected ion monitoring. The calibration curve for FAA in serum was linear over the range from 0.02 to 5 microg/ml, with limits of detection and quantification of 0.02 and 0.07 microg/ml, respectively. The method was also tested with spiked whole blood, urine, stomach contents and kidney samples. It was sufficiently reliable, reproducible and sensitive for use in routine forensic toxicology applications.

  20. RIA of PGFsub(2α) and PGE2 in biological samples of different origin: comparison with the mass fragmentographic technique

    International Nuclear Information System (INIS)

    Cattabeni, F.; Borghi, C.; Folco, G.C.; Nicosia, S.; Spagnuolo, C.

    1979-01-01

    The aim of this paper is to describe some results obtained measuring PGFsub(2α) and PGE 2 with bioassay, RIA and mass fragmentography in samples of different biological origin such as rat brain cortex and human urine of normal subjects and patients with Bartter's Syndrome. The results reported here clearly indicate that the assay of PGFsub(2α) and PGE 2 require an accurate validation with different analytical techniques. In fact, RIA of PGFsub(2α) gave different results if the samples were of different origin. It can be concluded that all the methods today available for PGs measurements need to be accurately validated utilizing different assays and that this validation is required everytime the sample matrix is changed. (Auth.)

  1. Determination of 2-Octanone in Biological Samples Using Liquid–Liquid Microextractions Followed by Gas Chromatography–Flame Ionization Detectio

    Directory of Open Access Journals (Sweden)

    Abolghasem Jouyban, Maryam Abbaspour, Mir Ali Farajzadeh, Maryam Khoubnasabjafari

    2017-06-01

    Full Text Available Background: Analysis of chemicals in biological fluids is required in many areas of medical sciences. Rapid, highly efficient, and reliable dispersive and air assisted liquid–liquid microextraction methods followed by gas chromatography-flame ionization detection were developed for the extraction, preconcentration, and determination of 2-octanone in human plasma and urine samples. Methods: Proteins of plasma samples are precipitated by adding methanol and urine sample is diluted with water prior to performing the microextraction procedure. Fine organic solvent droplets are formed by repeated suction and injection of the mixture of sample solution and extraction solvent into a test tube with a glass syringe. After extraction, phase separation is performed by centrifuging and the enriched analyte in the sedimented organic phase is determined by the separation system. The main factors influencing the extraction efficiency including extraction solvent type and volume, salt addition, pH, and extraction times are investigated. Results: Under the optimized conditions, the proposed method showed good precision (relative standard deviation less than 7%. Limit of detection and lower limit of quantification for 2-octanone were obtained in the range of 0.1–0.5 µg mL−1. The linear ranges were 0.5-500 and 0.5-200 µg mL−1 in plasma and urine, respectively (r2 ≥ 0.9995. Enrichment factors were in the range of 13-37. Good recoveries (55–86% were obtained for the spiked samples. Conclusion: Preconcentration methods coupled with GC analysis were developed and could be used to monitor 2-octanone in biological samples.

  2. Organochlorine pesticides in sediment and biological samples from the coastal lagoons of Nicaragua

    International Nuclear Information System (INIS)

    Montenegro, S.; Lacayo, M.; Picado, F.; Lopez, A.

    1999-01-01

    A study was carried out on the Pacific coast of Nicaragua to investigate the contamination of the coastal lagoons with residues of agricultural pesticides. Samples were taken during 1995 from the areas of Estero Real, Padre Ramos, Maderas Negras, Naranjo and Paso Caballos, and during 1996 from Aposentillo to Estero Barquito - Posoltega River. Analysis of the samples of sediment and aquatic life (fishes, oysters and bivalves) showed that they were contaminated with organochlorine pesticides. The pesticides found in the highest concentrations were toxaphene (1,734 μg.kg -1 ) and p,p-DDE (275 μg kg -1 ). These data indicate widespread contamination of the ecosystem with organochlorine pesticides in the main Pacific coastal lagoons of Nicaragua, resulting from intensive agricultural use of pesticides during the past decades. The contamination has been carried from the agricultural areas to the coastal lagoons by the rivers passing through the cultivated areas. (author)

  3. Trace determination of uranium and thorium in biological samples by radiochemical neutron activation analysis

    International Nuclear Information System (INIS)

    Benedik, Ljudmila; Repinc, Urska; Byrne, Anthony R.; Stegnar, Peter

    2002-01-01

    Radiochemical neutron activation analysis (RNAA) is an excellent method for determining uranium and thorium; it offers unique possibilities for their ultratrace analysis using selective radiochemical separations. Regarding the favourably sensitive nuclear characteristics of uranium and of thorium with respect to RNAA, but the different half-lives of their induced nuclides, two different approaches were used. In the first approach uranium and thorium were determined separately via 239 U, 239 Np and 233 Pa. In the second approach these elements were 239 239 233 determined simultaneously in a single sample using U and/or Np and Pa. Isolation of induced nuclides was based on separation by extraction and/or anion exchange chromatography. Chemical yields were measured in each sample aliquot using added 235 U, 238 Np and 231 Pa radioisotopic tracers. (author)

  4. Conceptual design and sampling procedures of the biological programme of NuukBasic

    DEFF Research Database (Denmark)

    Aastrup, Peter; Nymand, Josephine; Raundrup, Katrine

    Vegetation Index (NDVI). The fl ux of CO2 is measured in natural conditions as well as in manipulations simulating increased temperature, increased cloud cover, shorter growing season, and longer growing season. The effect of increased UV-B radiation on plant stress is studied by measuring chlorophyll fl...... uorescence in three series of plots. Arthropods are sampled by means of yellow pitfall traps as well as in window traps. Microarthropods are sampled in soil cores and extracted in an extractor by gradually heating up soil. The avifauna is monitored with special emphasis on passerine birds. Only few...... terrestrial mammals occur in the study area. All observations of mammals are recorded ad-hoc. Monitoring in lakes include ice cover, water chemistry, physical conditions, species composition of plankton, vegetation, bottom organisms and fi sh. Physical-chemical parameters, phytoplankton and zooplankton...

  5. Determination of technetium 99 in marine biological samples. Choice of a method

    International Nuclear Information System (INIS)

    Patti, Francois; Cappellini, Liliane; Jeanmaire, Lucien.

    1980-06-01

    The technique is easily carried out; it can be applied to the simultaneous analysis of several samples and requires no special instrumentation. Chemical yields, reproductibility and sensitivity are satisfying. The technique is based on the formation of pertechnetate ions un-entrained by hydroxides and retained on anionic resins; the nitric eluate is evaporated to dryness and its β - activity counted. The detection limit for 50 g of dry matter is 0.1 pCi.g -1 [fr

  6. Electrochemical Analysis of Antichemotherapeutic Drug Zanosar in Pharmaceutical and Biological Samples by Differential Pulse Polarography

    OpenAIRE

    Reddy, Chennupalle Nageswara; ReddyPrasad, Puthalapattu; Sreedhar, NeelamYughandhar

    2013-01-01

    The electrochemical reduction of zanosar was investigated systematically by direct current polarography, cyclic voltammetry, and differential pulse polarography (DPP). A simple DPP technique was proposed for the direct quantitative determination of anticancer drug zanosar in pharmaceutical formulation and spiked human urine samples for the first time. The reduction potential was −0.28 V versus Ag/AgCl with a hanging mercury drop electrode in Britton-Robinson buffer as supporting electrolyte. ...

  7. Surface plasmon resonance: advances of label-free approaches in the analysis of biological samples

    Czech Academy of Sciences Publication Activity Database

    Riedel, Tomáš; Majek, P.; Rodriguez-Emmenegger, Cesar; Brynda, Eduard

    2014-01-01

    Roč. 6, č. 24 (2014), s. 3325-3336 ISSN 1757-6180 R&D Projects: GA ČR(CZ) GBP205/12/G118; GA MŠk(CZ) EE2.3.30.0029; GA MŠk(CZ) ED1.1.00/02.0109 Institutional support: RVO:61389013 Keywords : surface plasmon resonance sensors * polymer brushes * human serum samples Subject RIV: CE - Biochemistry Impact factor: 3.003, year: 2014

  8. Label-free quantification of Tacrolimus in biological samples by atomic force microscopy

    International Nuclear Information System (INIS)

    Menotta, Michele; Biagiotti, Sara; Streppa, Laura; Rossi, Luigia; Magnani, Mauro

    2015-01-01

    Highlights: • Tacrolimus is a potent immunosuppressant drug that has to be continually monitored. • We present an atomic force microscope approach for quantification of Tacrolimus in blood samples. • Detection and quantification have been successfully achieved. - Abstract: In the present paper we describe an atomic force microscopy (AFM)-based method for the quantitative analysis of FK506 (Tacrolimus) in whole blood (WB) samples. Current reference methods used to quantify this immunosuppressive drug are based on mass spectrometry. In addition, an immunoenzymatic assay (ELISA) has been developed and is widely used in clinic, even though it shows a small but consistent overestimation of the actual drug concentration when compared with the mass spectrometry method. The AFM biosensor presented herein utilises the endogen drug receptor, FKBP12, to quantify Tacrolimus levels. The biosensor was first assayed to detect the free drug in solution, and subsequently used for the detection of Tacrolimus in blood samples. The sensor was suitable to generate a dose–response curve in the full range of clinical drug monitoring. A comparison with the clinically tested ELISA assay is also reported

  9. Electrochemical analysis of antichemotherapeutic drug zanosar in pharmaceutical and biological samples by differential pulse polarography.

    Science.gov (United States)

    Reddy, Chennupalle Nageswara; Reddyprasad, Puthalapattu; Sreedhar, Neelamyughandhar

    2013-01-01

    The electrochemical reduction of zanosar was investigated systematically by direct current polarography, cyclic voltammetry, and differential pulse polarography (DPP). A simple DPP technique was proposed for the direct quantitative determination of anticancer drug zanosar in pharmaceutical formulation and spiked human urine samples for the first time. The reduction potential was -0.28 V versus Ag/AgCl with a hanging mercury drop electrode in Britton-Robinson buffer as supporting electrolyte. The dependence of the intensities of currents and potentials on pH, concentration, scan rate, deposition time, and nature of the supporting electrolyte was investigated. The calibration curve was found to be linear with the following equation: y = 0.4041x + 0.012, with a correlation coefficient of 0.992 (R (2)) over a concentration range from 1.0 × 10(-7) M to 1.0 × 10(-3) M. In the present investigation, the achieved limit of detection (LOD) and limit of quantization (LQD) were 7.42 × 10(-8) M and 2.47 × 10(-8) M; respectively. Excipients did not interfere with the determination of zanosar in pharmaceutical formulation and spiked urine samples. Precision and accuracy of the developed method were checked by recovery studies in pharmaceutical formulation and spiked human urine samples.

  10. Electrochemical Analysis of Antichemotherapeutic Drug Zanosar in Pharmaceutical and Biological Samples by Differential Pulse Polarography

    Directory of Open Access Journals (Sweden)

    Chennupalle Nageswara Reddy

    2013-01-01

    Full Text Available The electrochemical reduction of zanosar was investigated systematically by direct current polarography, cyclic voltammetry, and differential pulse polarography (DPP. A simple DPP technique was proposed for the direct quantitative determination of anticancer drug zanosar in pharmaceutical formulation and spiked human urine samples for the first time. The reduction potential was −0.28 V versus Ag/AgCl with a hanging mercury drop electrode in Britton-Robinson buffer as supporting electrolyte. The dependence of the intensities of currents and potentials on pH, concentration, scan rate, deposition time, and nature of the supporting electrolyte was investigated. The calibration curve was found to be linear with the following equation: y=0.4041x+0.012, with a correlation coefficient of 0.992 (R2 over a concentration range from 1.0×10-7 M to 1.0×10-3 M. In the present investigation, the achieved limit of detection (LOD and limit of quantization (LQD were 7.42×10-8 M and 2.47×10-8 M; respectively. Excipients did not interfere with the determination of zanosar in pharmaceutical formulation and spiked urine samples. Precision and accuracy of the developed method were checked by recovery studies in pharmaceutical formulation and spiked human urine samples.

  11. Experimental set up for the irradiation of biological samples and nuclear track detectors with UV C.

    Science.gov (United States)

    Portu, Agustina Mariana; Rossini, Andrés Eugenio; Gadan, Mario Alberto; Bernaola, Omar Alberto; Thorp, Silvia Inés; Curotto, Paula; Pozzi, Emiliano César Cayetano; Cabrini, Rómulo Luis; Martin, Gisela Saint

    2016-01-01

    In this work we present a methodology to produce an "imprint" of cells cultivated on a polycarbonate detector by exposure of the detector to UV C radiation. The distribution and concentration of (10)B atoms in tissue samples coming from BNCT (Boron Neutron Capture Therapy) protocols can be determined through the quantification and analysis of the tracks forming its autoradiography image on a nuclear track detector. The location of boron atoms in the cell structure could be known more accurately by the simultaneous observation of the nuclear tracks and the sample image on the detector. A UV C irradiator was constructed. The irradiance was measured along the lamp direction and at different distances. Melanoma cells were cultured on polycarbonate foils, incubated with borophenylalanine, irradiated with thermal neutrons and exposed to UV C radiation. The samples were chemically attacked with a KOH solution. A uniform irradiation field was established to expose the detector foils to UV C light. Cells could be seeded on the polycarbonate surface. Both imprints from cells and nuclear tracks were obtained after chemical etching. It is possible to yield cellular imprints in polycarbonate. The nuclear tracks were mostly present inside the cells, indicating a preferential boron uptake.

  12. Analysis of Biological Samples Using Paper Spray Mass Spectrometry: An Investigation of Impacts by the Substrates, Solvents and Elution Methods.

    Science.gov (United States)

    Ren, Yue; Wang, He; Liu, Jiangjiang; Zhang, Zhiping; McLuckey, Morgan N; Ouyang, Zheng

    2013-10-01

    Paper spray has been developed as a fast sampling ionization method for direct analysis of raw biological and chemical samples using mass spectrometry (MS). Quantitation of therapeutic drugs in blood samples at high accuracy has also been achieved using paper spray MS without traditional sample preparation or chromatographic separation. The paper spray ionization is a process integrated with a fast extraction of the analyte from the raw sample by a solvent, the transport of the extracted analytes on the paper, and a spray ionization at the tip of the paper substrate with a high voltage applied. In this study, the influence on the analytical performance by the solvent-substrate systems and the selection of the elution methods was investigated. The protein hemoglobin could be observed from fresh blood samples on silanized paper or from dried blood spots on silica-coated paper. The on-paper separation of the chemicals during the paper spray was characterized through the analysis of a mixture of the methyl violet 2B and methylene blue. The mode of applying the spray solvent was found to have a significant impact on the separation. The results in this study led to a better understanding of the analyte elution, on-paper separation, as well as the ionization processes of the paper spray. This study also help to establish a guideline for optimizing the analytical performance of paper spray for direct analysis of target analytes using mass spectrometry.

  13. Development of a micro-XRF system for biological samples based on proton-induced quasimonochromatic X-rays

    Energy Technology Data Exchange (ETDEWEB)

    Ploykrachang, K., E-mail: ploykrachang.k.aa@m.titech.ac.jp [Research Laboratory for Nuclear Reactors, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku, Tokyo 152-8550 (Japan); Hasegawa, J. [Department of Energy Sciences, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, 4259 Nagatsuta-cho, Midori-ku, Yokohama 226-8502 (Japan); Kondo, K.; Fukuda, H.; Oguri, Y. [Research Laboratory for Nuclear Reactors, Tokyo Institute of Technology, 2-12-1 Ookayama, Meguro-ku, Tokyo 152-8550 (Japan)

    2014-07-15

    We have developed a micro-XRF system based on a proton-induced quasimonochromatic X-ray (QMXR) microbeam for in vivo measurement of biological samples. A 2.5-MeV proton beam impinged normally on a Cu foil target that was slightly thicker than the proton range. The emitted QMXR behind the Cu target was focused with a polycapillary X-ray half lens. For application to analysis of wet or aquatic samples, we prepared a QMXR beam with an incident angle of 45° with respect to the horizontal plane by using a dipole magnet in order to bend the primary proton beam downward by 45°. The focal spot size of the QMXR microbeam on a horizontal sample surface was evaluated to be 250 × 350 μm by a wire scanning method. A microscope camera with a long working distance was installed perpendicular to the sample surface to identify the analyzed position on the sample. The fluorescent radiation from the sample was collected by a Si-PIN photodiode X-ray detector. Using the setup above, we were able to successfully measure the accumulation and distribution of Co in the leaves of a free-floating aquatic plant on a dilute Co solution surface.

  14. Applications of High Resolution Laser Induced Breakdown Spectroscopy for Environmental and Biological Samples

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Madhavi Z [ORNL; Labbe, Nicole [ORNL; Wagner, Rebekah J. [Pennsylvania State University, University Park, PA

    2013-01-01

    This chapter details the application of LIBS in a number of environmental areas of research such as carbon sequestration and climate change. LIBS has also been shown to be useful in other high resolution environmental applications for example, elemental mapping and detection of metals in plant materials. LIBS has also been used in phytoremediation applications. Other biological research involves a detailed understanding of wood chemistry response to precipitation variations and also to forest fires. A cross-section of Mountain pine (pinceae Pinus pungen Lamb.) was scanned using a translational stage to determine the differences in the chemical features both before and after a fire event. Consequently, by monitoring the elemental composition pattern of a tree and by looking for abrupt changes, one can reconstruct the disturbance history of a tree and a forest. Lastly we have shown that multivariate analysis of the LIBS data is necessary to standardize the analysis and correlate to other standard laboratory techniques. LIBS along with multivariate statistical analysis makes it a very powerful technology that can be transferred from laboratory to field applications with ease.

  15. Demonstration Exercise of a Validated Sample Collection Method for Powders Suspected of Being Biological Agents in Georgia 2006

    International Nuclear Information System (INIS)

    Marsh, B.

    2007-01-01

    August 7, 2006 the state of Georgia conducted a collaborative sampling exercise between the Georgia National Guard 4th Civil Support Team Weapons of Mass Destruction (CST-WMD) and the Georgia Department of Human Resources Division of Public Health demonstrating a recently validated bulk powder sampling method. The exercise was hosted at the Federal Law Enforcement Training Center (FLETC) at Glynn County, Georgia and involved the participation of the Georgia Emergency Management Agency (GEMA), Georgia National Guard, Georgia Public Health Laboratories, the Federal Bureau of Investigation Atlanta Office, Georgia Coastal Health District, and the Glynn County Fire Department. The purpose of the exercise was to demonstrate a recently validated national sampling standard developed by the American Standards and Test Measures (ASTM) International; ASTM E2458 S tandard Practice for Bulk Sample Collection and Swab Sample Collection of Visible Powders Suspected of Being Biological Agents from Nonporous Surfaces . The intent of the exercise was not to endorse the sampling method, but to develop a model for exercising new sampling methods in the context of existing standard operating procedures (SOPs) while strengthening operational relationships between response teams and analytical laboratories. The exercise required a sampling team to respond real-time to an incident cross state involving a clandestine bio-terrorism production lab found within a recreational vehicle (RV). Sample targets consisted of non-viable gamma irradiated B. anthracis Sterne spores prepared by Dugway Proving Ground. Various spore concentration levels were collected by the ASTM method, followed by on- and off-scene analysis utilizing the Center for Disease Control (CDC) Laboratory Response Network (LRN) and National Guard Bureau (NGB) CST mobile Analytical Laboratory Suite (ALS) protocols. Analytical results were compared and detailed surveys of participant evaluation comments were examined. I will

  16. A comparison of sample preparation strategies for biological tissues and subsequent trace element analysis using LA-ICP-MS.

    Science.gov (United States)

    Bonta, Maximilian; Török, Szilvia; Hegedus, Balazs; Döme, Balazs; Limbeck, Andreas

    2017-03-01

    Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is one of the most commonly applied methods for lateral trace element distribution analysis in medical studies. Many improvements of the technique regarding quantification and achievable lateral resolution have been achieved in the last years. Nevertheless, sample preparation is also of major importance and the optimal sample preparation strategy still has not been defined. While conventional histology knows a number of sample pre-treatment strategies, little is known about the effect of these approaches on the lateral distributions of elements and/or their quantities in tissues. The technique of formalin fixation and paraffin embedding (FFPE) has emerged as the gold standard in tissue preparation. However, the potential use for elemental distribution studies is questionable due to a large number of sample preparation steps. In this work, LA-ICP-MS was used to examine the applicability of the FFPE sample preparation approach for elemental distribution studies. Qualitative elemental distributions as well as quantitative concentrations in cryo-cut tissues as well as FFPE samples were compared. Results showed that some metals (especially Na and K) are severely affected by the FFPE process, whereas others (e.g., Mn, Ni) are less influenced. Based on these results, a general recommendation can be given: FFPE samples are completely unsuitable for the analysis of alkaline metals. When analyzing transition metals, FFPE samples can give comparable results to snap-frozen tissues. Graphical abstract Sample preparation strategies for biological tissues are compared with regard to the elemental distributions and average trace element concentrations.

  17. Focal molography is a new method for the in situ analysis of molecular interactions in biological samples

    Science.gov (United States)

    Gatterdam, Volker; Frutiger, Andreas; Stengele, Klaus-Peter; Heindl, Dieter; Lübbers, Thomas; Vörös, Janos; Fattinger, Christof

    2017-11-01

    Focal molography is a next-generation biosensor that visualizes specific biomolecular interactions in real time. It transduces affinity modulation on the sensor surface into refractive index modulation caused by target molecules that are bound to a precisely assembled nanopattern of molecular recognition sites, termed the 'mologram'. The mologram is designed so that laser light is scattered at specifically bound molecules, generating a strong signal in the focus of the mologram via constructive interference, while scattering at nonspecifically bound molecules does not contribute to the effect. We present the realization of molograms on a chip by submicrometre near-field reactive immersion lithography on a light-sensitive monolithic graft copolymer layer. We demonstrate the selective and sensitive detection of biomolecules, which bind to the recognition sites of the mologram in various complex biological samples. This allows the label-free analysis of non-covalent interactions in complex biological samples, without a need for extensive sample preparation, and enables novel time- and cost-saving ways of performing and developing immunoassays for diagnostic tests.

  18. Is it ethical to prevent secondary use of stored biological samples and data derived from consenting research participants? The case of Malawi.

    Science.gov (United States)

    Mungwira, Randy G; Nyangulu, Wongani; Misiri, James; Iphani, Steven; Ng'ong'ola, Ruby; Chirambo, Chawanangwa M; Masiye, Francis; Mfutso-Bengo, Joseph

    2015-12-02

    This paper discusses the contentious issue of reuse of stored biological samples and data obtained from research participants in past clinical research to answer future ethical and scientifically valid research questions. Many countries have regulations and guidelines that guide the use and exportation of stored biological samples and data. However, there are variations in regulations and guidelines governing the reuse of stored biological samples and data in Sub-Saharan Africa including Malawi. The current research ethics regulations and guidelines in Malawi do not allow indefinite storage and reuse of biological samples and data for future unspecified research. This comes even though the country has managed to answer pertinent research questions using stored biological samples and data. We acknowledge the limited technical expertise and equipment unavailable in Malawi that necessitates exportation of biological samples and data and the genuine concern raised by the regulatory authorities about the possible exploitation of biological samples and data by researchers. We also acknowledge that Malawi does not have bio-banks for storing biological samples and data for future research purposes. This creates room for possible exploitation of biological samples and data collected from research participants in primary research projects in Malawi. However, research ethics committees require completion and approval of material transfer agreements and data transfer agreements for biological samples and data collected for research purposes respectively and this requirement may partly address the concern raised by the regulatory authorities. Our concern though is that there is no such requirement for biological samples and data collected from patients for clinical or diagnostic purposes. In conclusion, we propose developing a medical data and material transfer agreement for biological samples and data collected from patients for clinical or diagnostic purposes in both public

  19. Determination of iodine in biological samples by neutron activation analysis (NAA)

    International Nuclear Information System (INIS)

    Geetha, P.V.; Karunakara, N.; Prabhu, Ujwal; Yashodhara, I.; Ravi, P.M.; Sudhakar, J.; Ajith, Nicy; Swain, K.K.; Verma, R.; Reddy, A.V.R.; Acharya, R.

    2010-01-01

    During normal operating conditions of a nuclear reactor, the release of radionuclides to the environment will be extremely low and well within the limits. Radioiodine ( 131 I) is one of the radionuclides likely to get released into the atmosphere in case of a reactor accident. During the short initial phase of release of radioactivity, 131 I is rapidly transferred to milk, leading to significant thyroid dose to those consuming milk, especially infant and children. Hence, studies on Iodine transfer through grass-cow-milk is very important. Extensive studies on transfer for 131 I through grass-cow-milk pathway after Chernobyl accident has been reported. But, under normal operational conditions of the power reactor, 131 I is not present in measurable concentration in environmental matrices of a nuclear power generating station. Stable iodine is present in all environmental samples and from the concentration of stable iodine in grass and milk, one can estimate the transfer factor. The measurement of stable iodine in environmental sample is very challenging because of its extremely low concentration. Neutron activation analysis can be used for estimation of stable iodine in the environment after suitably optimizing the condition to minimize interferences. A method has been developed based on thermal neutron activation analysis (NAA) to estimate the iodine concentration present in grass and cow milk

  20. Enhanced methods for unbiased deep sequencing of Lassa and Ebola RNA viruses from clinical and biological samples.

    Science.gov (United States)

    Matranga, Christian B; Andersen, Kristian G; Winnicki, Sarah; Busby, Michele; Gladden, Adrianne D; Tewhey, Ryan; Stremlau, Matthew; Berlin, Aaron; Gire, Stephen K; England, Eleina; Moses, Lina M; Mikkelsen, Tarjei S; Odia, Ikponmwonsa; Ehiane, Philomena E; Folarin, Onikepe; Goba, Augustine; Kahn, S Humarr; Grant, Donald S; Honko, Anna; Hensley, Lisa; Happi, Christian; Garry, Robert F; Malboeuf, Christine M; Birren, Bruce W; Gnirke, Andreas; Levin, Joshua Z; Sabeti, Pardis C

    2014-01-01

    We have developed a robust RNA sequencing method for generating complete de novo assemblies with intra-host variant calls of Lassa and Ebola virus genomes in clinical and biological samples. Our method uses targeted RNase H-based digestion to remove contaminating poly(rA) carrier and ribosomal RNA. This depletion step improves both the quality of data and quantity of informative reads in unbiased total RNA sequencing libraries. We have also developed a hybrid-selection protocol to further enrich the viral content of sequencing libraries. These protocols have enabled rapid deep sequencing of both Lassa and Ebola virus and are broadly applicable to other viral genomics studies.

  1. Advancements in mass spectrometry for biological samples: Protein chemical cross-linking and metabolite analysis of plant tissues

    Energy Technology Data Exchange (ETDEWEB)

    Klein, Adam [Iowa State Univ., Ames, IA (United States)

    2015-01-01

    This thesis presents work on advancements and applications of methodology for the analysis of biological samples using mass spectrometry. Included in this work are improvements to chemical cross-linking mass spectrometry (CXMS) for the study of protein structures and mass spectrometry imaging and quantitative analysis to study plant metabolites. Applications include using matrix-assisted laser desorption/ionization-mass spectrometry imaging (MALDI-MSI) to further explore metabolic heterogeneity in plant tissues and chemical interactions at the interface between plants and pests. Additional work was focused on developing liquid chromatography-mass spectrometry (LC-MS) methods to investigate metabolites associated with plant-pest interactions.

  2. Magnetic restricted-access microspheres for extraction of adrenaline, dopamine and noradrenaline from biological samples

    International Nuclear Information System (INIS)

    Xiao, Deli; Liu, Shubo; Liang, Liyun; Bi, Yanping

    2016-01-01

    Epoxy propyl bonded magnetic microspheres were prepared by atomic layer deposition using Fe 3 O 4 -SiO 2 microspheres as a core support material. Then, a restricted-access magnetic sorbent was prepared that contains diol groups on the external surface and m-aminophenylboronic acid groups on the internal surface. This kind of microspheres achieved excellent specific adsorption of the ortho-dihydroxy compounds (dopamine, adrenaline and noradrenaline). Following desorption with sorbitol, the ortho-dihydroxy compounds were quantified by HPLC. The limits of detection for dopamine, adrenaline and noradrenaline were 0.074, 0.053 and 0.095 μg mL −1 , respectively. Recoveries from spiked mice serum samples range from 80.2 to 89.1 %. (author)

  3. Optimization of a radiochemistry method for plutonium determination in biological samples

    International Nuclear Information System (INIS)

    Cerchetti, Maria L.; Arguelles, Maria G.

    2005-01-01

    Plutonium has been widely used for civilian an military activities. Nevertheless, the methods to control work exposition have not evolved in the same way, remaining as one of the major challengers for the radiological protection practice. Due to the low acceptable incorporation limit, the usual determination is based on indirect methods in urine samples. Our main objective was to optimize a technique used to monitor internal contamination of workers exposed to Plutonium isotopes. Different parameters were modified and their influence on the three steps of the method was evaluated. Those which gave the highest yield and feasibility were selected. The method involves: 1-) Sample concentration (coprecipitation); 2-) Plutonium purification; and 3-) Source preparation by electrodeposition. On the coprecipitation phase, changes on temperature and concentration of the carrier were evaluated. On the ion-exchange separation, changes on the type of the resin, elution solution for hydroxylamine (concentration and volume), length and column recycle were evaluated. Finally, on the electrodeposition phase, we modified the following: electrolytic solution, pH and time. Measures were made by liquid scintillation counting and alpha spectrometry (PIPS). We obtained the following yields: 88% for coprecipitation (at 60 C degree with 2 ml of CaHPO 4 ), 71% for ion-exchange (resins AG 1x8 Cl - 100-200 mesh, hydroxylamine 0.1N in HCl 0.2N as eluent, column between 4.5 and 8 cm), and 93% for electrodeposition (H 2 SO 4 -NH 4 OH, 100 minutes and pH from 2 to 2.8). The expand uncertainty was 30% (NC 95%), the decision threshold (Lc) was 0.102 Bq/L and the minimum detectable activity was 0.218 Bq/L of urine. We obtained an optimized method to screen workers exposed to Plutonium. (author)

  4. k0-INAA application at IPEN Neutron Activation Laboratory by using the k0-IAEA program: biological sample analysis

    International Nuclear Information System (INIS)

    Puerta, Daniel Correa

    2013-01-01

    The results obtained in the application of the k 0 -standardization method at LAN-IPEN for biological matrices analysis, by using the k 0 -IAEA software, provided by the International Atomic Energy Agency (IAEA), are presented. The flux parameters f and a of the IEA-R1 reactor were determined for the pneumatic irradiation facility and for one selected irradiation position, 24B/shelf2, for short and long irradiations, respectively. In order to obtain these parameters, the bare triple-monitor method with 197 Au- 96 Zr- 94 Zr was used. In order to evaluate the accuracy and precision of the methodology, the biological reference materials Peach Leaves (NIST SRM 1547), Mixed Polish Herbs (INCT-MPH-2) e Tomato Leaves (NIST SRM 1573a) were analyzed. The statistical criteria Relative Errors (bias, %), Coefficient of Variation (CV) and U-score were applied to the obtained results (mean of six replicates). The relative errors (bias, %) in relation to certified values, were, for most elements, in the range of 0 e 30. The Coefficients of Variation were below 20%, showing a good reproducibility of the results. The U-score test showed that all results, except Na in Peach Leaves and in Tomato Leaves, were within 95% confidence interval. These results point out to a promising use of the k 0 -INAA method at LAN-IPEN for biological sample analysis. (author)

  5. Measurement of total CO2 in microliter samples of urine and other biological fluids using infrared detection of CO2.

    Science.gov (United States)

    Trepiccione, Francesco; Iena, Francesco Maria; Catalini, Laura; Carpi, Francesco Martino; Koed, Mogens; Frische, Sebastian

    2017-10-01

    The purpose of this study is to describe a low-cost and simply made instrument capable of measuring the total CO 2 content of microliter volumes of biological fluids utilizing a commercially available CO 2 sensor based on a NDIR detector. The described instrument is based on transformation of dissolved HCO 3 - to CO 2 by acidification and subsequent measurement of the produced CO 2 . The instrument has a linear response in the range 0.025-10 μmol HCO 3 - , which enables measurements in fresh urine and plasma samples down to 5 μl. The values from plasma were compared to measurements made on 65 μl whole blood in an automatic blood gas analyzer and found not to differ significantly. Compared to currently commercially available instruments applying the same principles to measure total CO 2 , this study provides a simple and robust alternative which even can be used on smaller sample volumes.

  6. High-resolution, high-transmission soft x-ray spectrometer for the study of biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Fuchs, Oliver; Weinhardt, L.; Blum, M.; Welgand, M.; Umbach, E.; Bar, M.; Heske, C.; Denlinger, J.; Chuang, Y.-D.; McKinney, W.; Hussain, Z.; Gullikson, E.; Jones, M.; Batson, P.; Nelles, B.; Follath, R.

    2009-06-11

    We present a variable line-space grating spectrometer for soft s-rays that coverst the photon energy range between 130 and 650 eV. The optical design is based on the Hettrick-Underwood principle and tailored to synchrotron-based studies of radiation-sensitive biological samples. The spectrometer is able to record the entire spectral range in one shot, i.e., without any mechanical motion, at a resolving power of 1200 or better. Despite is slitless design, such a resolving power can be achieved for a source spot as large as (30 x 3000) micrometers squared, which is important for keeping beam damage effects in radiation-sensitive samples low. The high spectrometer efficiency allows recording of comprehensive two-dimensional resonant inelastic soft x-ray scatters (RIXS) maps with good statistics within several minutes. This is exemplarily demonstrated for a RIXS map of highly oriented pyrolytic graphite, which was taken with 10 min.

  7. A bench-top K X-ray fluorescence system for quantitative measurement of gold nanoparticles for biological sample diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Ricketts, K., E-mail: k.ricketts@ucl.ac.uk [Division of Surgery and Interventional Sciences, University College London, Royal Free Campus, Rowland Hill Street, London NW3 2PF (United Kingdom); Guazzoni, C.; Castoldi, A. [Dipartimento di Elettronica, Informazione e Bioingegneria Politecnico di Milano and INFN, Sezione di Milano P.za Leonardo da Vinci, 32-20133 Milano (Italy); Royle, G. [Department of Medical Physics and Bioengineering, University College London, Malet Place Engineering Building, Gower Street, London WC1E 6BT (United Kingdom)

    2016-04-21

    Gold nanoparticles can be targeted to biomarkers to give functional information on a range of tumour characteristics. X-ray fluorescence (XRF) techniques offer potential quantitative measurement of the distribution of such heavy metal nanoparticles. Biologists are developing 3D tissue engineered cellular models on the centimetre scale to optimise targeting techniques of nanoparticles to a range of tumour characteristics. Here we present a high energy bench-top K-X-ray fluorescence system designed for sensitivity to bulk measurement of gold nanoparticle concentration for intended use in such thick biological samples. Previous work has demonstrated use of a L-XRF system in measuring gold concentrations but being a low energy technique it is restricted to thin samples or superficial tumours. The presented system comprised a high purity germanium detector and filtered tungsten X-ray source, capable of quantitative measurement of gold nanoparticle concentration of thicker samples. The developed system achieved a measured detection limit of between 0.2 and 0.6 mgAu/ml, meeting specifications of biologists and being approximately one order of magnitude better than the detection limit of alternative K-XRF nanoparticle detection techniques. The scatter-corrected K-XRF signal of gold was linear with GNP concentrations down to the detection limit, thus demonstrating potential in GNP concentration quantification. The K-XRF system demonstrated between 5 and 9 times less sensitivity than a previous L-XRF bench-top system, due to a fundamental limitation of lower photoelectric interaction probabilities at higher K-edge energies. Importantly, the K-XRF technique is however less affected by overlying thickness, and so offers future potential in interrogating thick biological samples.

  8. Polybrominated diphenyl ethers in water, sediment, soil, and biological samples from different industrial areas in Zhejiang, China

    International Nuclear Information System (INIS)

    Wang, Junxia; Lin, Zhenkun; Lin, Kuangfei; Wang, Chunyan; Zhang, Wei; Cui, Changyuan; Lin, Junda; Dong, Qiaoxiang; Huang, Changjiang

    2011-01-01

    Highlights: ► We examined PBDE concentrations in various matrices from different industrial areas. ► Elevated PBDE levels were found in areas with low-voltage electrical manufactures. ► Areas with e-waste recycling activities also had higher PBDE concentrations. ► PBDE content and composition in water samples varied from one area to another. ► PBDE composition in sediment/soil and biological samples was predominated by BDE-209. - Abstract: Polybrominated diphenyl ethers (PBDEs) have been used extensively in electrical and electronic products, but little is known about their distribution in the environment surrounding the manufacturing factories. This study reports PBDE contamination in various matrices from the location (Liushi, Zhejiang province) that produces more than 70% of the low-voltage electrical appliances in China. Additionally, PBDE contamination was compared with other industries such as the e-waste recycling business (Fengjiang) in the same region. Specifically, we measured seven PBDE congeners (BDEs – 47, 99, 100, 153, 154, 183, and 209) in water, sediment, soil, plant, and animal tissues from four different areas in this region. The present study revealed elevated PBDE concentrations in all matrices collected from Liushi and Fengjiang in comparison with highly industrialized areas without significant PBDE contamination sources. In water samples, there were large variations of PBDE content and composition across different areas. In sediment/soil and biological samples, BDE-209 was the predominant congener and this could be due to the abundant usage of deca-BDE mixtures in China. Our findings provide the very first data on PBDE contamination in the local environments surrounding the electronics industry, and also reveal widespread PBDE contamination in highly industrialized coastal regions of China.

  9. Radioreceptor assay for analysis of fentanyl and its analogs in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Alburges, M.E.

    1988-01-01

    The assay is based on the competition of these drugs with ({sup 3}H) fentanyl for opioid receptors in membrane preparations of rat forebrain in vitro. The binding in stereospecific, reversible and saturable. Scatchard plots of saturation suggest the presence of high and low affinity binding sites. Morphine and hydromorphone complete with ({sup 3}H)fentanyl for the opioid receptor, but other morphine-like compounds were relatively weak displacers of ({sup 3}H)fentanyl. Many other commonly abused drugs do not compete with ({sup 3}H)fentanyl for the opioid receptors. Urine samples from animals injected with fentanyl, ({plus minus})-cis-3-methylfentanyl, alpha-methylfentanyl, butyrylfentanyl and benzylfentanyl were analyzed by radioreceptor assay, radioimmunoassay, and gas chromatography/mass spectrometry. Urinary analysis of fentanyl showed a good correlation with these three methods; however, discrepancies were observed in the analysis of fentanyl analogs. This radioreceptor assay is well-suited as an initial assay for the detection of active analogs of fentanyl in urine with good correlation with other techniques in the analysis of fentanyl; however, there is substantial disagreement between techniques in the quantitation of fentanyl analogs. The implications of these discrepancies are discussed.

  10. Visual detection of Brucella in bovine biological samples using DNA-activated gold nanoparticles.

    Directory of Open Access Journals (Sweden)

    Dheeraj Pal

    Full Text Available Brucellosis is a bacterial disease, which, although affecting cattle primarily, has been associated with human infections, making its detection an important challenge. The existing gold standard diagnosis relies on the culture of bacteria which is a lengthy and costly process, taking up to 45 days. New technologies based on molecular diagnosis have been proposed, either through dip-stick, immunological assays, which have limited specificity, or using nucleic acid tests, which enable to identify the pathogen, but are impractical for use in the field, where most of the reservoir cases are located. Here we demonstrate a new test based on hybridization assays with metal nanoparticles, which, upon detection of a specific pathogen-derived DNA sequence, yield a visual colour change. We characterise the components used in the assay with a range of analytical techniques and show sensitivities down to 1000 cfu/ml for the detection of Brucella. Finally, we demonstrate that the assay works in a range of bovine samples including semen, milk and urine, opening up the potential for its use in the field, in low-resource settings.

  11. Rapid determination of amino acids in biological samples using a monolithic silica column.

    Science.gov (United States)

    Song, Yanting; Funatsu, Takashi; Tsunoda, Makoto

    2012-05-01

    A high-performance liquid chromatography method in which fluorescence detection is used for the simultaneous determination of 21 amino acids is proposed. Amino acids were derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) and then separated on a monolithic silica column (MonoClad C18-HS, 150 mm×3 mm i.d.). A mixture of 25 mM citrate buffer containing 25 mM sodium perchlorate (pH 5.5) and acetonitrile was used as the mobile phase. We found that the most significant factor in the separation was temperature, and a linear temperature gradient from 30 to 49°C was used to control the column temperature. The limits of detection and quantification for all amino acids ranged from 3.2 to 57.2 fmol and 10.8 to 191 fmol, respectively. The calibration curves for the NBD-amino acid had good linearity within the range of 40 fmol to 40 pmol when 6-aminocaproic acid was used as an internal standard. Using only conventional instruments, the 21 amino acids could be analyzed within 10 min. This method was found to be suitable for the quantification of the contents of amino acids in mouse plasma and adrenal gland samples.

  12. Electrokinetic migration across artificial liquid membranes. New concept for rapid sample preparation of biological fluids.

    Science.gov (United States)

    Pedersen-Bjergaard, Stig; Rasmussen, Knut Einar

    2006-03-24

    Basic drug substances were transported across a thin artificial organic liquid membrane by the application of 300 V d.c. From a 300 microl aqueous donor compartment (containing 10 mM HCl), the drugs migrated through a 200 microm artificial liquid membrane of 2-nitrophenyl octyl ether immobilized in the pores of a polypropylene hollow fiber, and into a 30 microl aqueous acceptor solution of 10 mM HCl inside the lumen of the hollow fiber. The transport was forced by an electrical potential difference sustained over the liquid membrane, resulting in electrokinetic migration of drug substances from the donor compartment to the acceptor solution. Within 5 min of operation at 300 V, pethidine, nortriptyline, methadone, haloperidol, and loperamide were extracted with recoveries in the range 70-79%, which corresponded to enrichments in the range 7.0-7.9. The chemical composition of the organic liquid membrane strongly affected the permeability, and may serve as an efficient tool for controlling the transport selectivity. Water samples, human plasma, and human urine were successfully processed, and in light of the present report, electrokinetic migration across thin artificial liquid membranes may be an interesting tool for future isolation within chemical analysis.

  13. Radioreceptor assay for analysis of fentanyl and its analogs in biological samples

    International Nuclear Information System (INIS)

    Alburges, M.E.

    1988-01-01

    The assay is based on the competition of these drugs with [ 3 H] fentanyl for opioid receptors in membrane preparations of rat forebrain in vitro. The binding in stereospecific, reversible and saturable. Scatchard plots of saturation suggest the presence of high and low affinity binding sites. Morphine and hydromorphone complete with [ 3 H]fentanyl for the opioid receptor, but other morphine-like compounds were relatively weak displacers of [ 3 H]fentanyl. Many other commonly abused drugs do not compete with [ 3 H]fentanyl for the opioid receptors. Urine samples from animals injected with fentanyl, (±)-cis-3-methylfentanyl, alpha-methylfentanyl, butyrylfentanyl and benzylfentanyl were analyzed by radioreceptor assay, radioimmunoassay, and gas chromatography/mass spectrometry. Urinary analysis of fentanyl showed a good correlation with these three methods; however, discrepancies were observed in the analysis of fentanyl analogs. This radioreceptor assay is well-suited as an initial assay for the detection of active analogs of fentanyl in urine with good correlation with other techniques in the analysis of fentanyl; however, there is substantial disagreement between techniques in the quantitation of fentanyl analogs. The implications of these discrepancies are discussed

  14. Low cost label-free live cell imaging for biological samples

    Science.gov (United States)

    Seniya, C.; Towers, C. E.; Towers, D. P.

    2017-02-01

    This paper reports the progress to develop a practical phase measuring microscope offering new capabilities in terms of phase measurement accuracy and quantification of cell:cell interactions over the longer term. A novel, low cost phase interference microscope for imaging live cells (label-free) is described. The method combines the Zernike phase contrast approach with a dual mirror design to enable phase modulation between the scattered and un-scattered optical fields. Two designs are proposed and demonstrated, one of which retains the common path nature of Zernike's original microscopy concept. In both setups the phase shift is simple to control via a piezoelectric driven mirror in the back focal plane of the imaging system. The approach is significantly cheaper to implement than those based on spatial light modulators (SLM) at approximately 20% of the cost. A quantitative assessment of the performance of a set of phase shifting algorithms is also presented, specifically with regard to broad bandwidth illumination in phase contrast microscopy. The simulation results show that the phase measurement accuracy is strongly dependent on the algorithm selected and the optical path difference in the sample.

  15. Perfluorooctanesulfonate and related fluorochemicals in biological samples from the north coast of Colombia

    International Nuclear Information System (INIS)

    Olivero-Verbel, Jesus; Tao, Lin; Johnson-Restrepo, Boris; Guette-Fernandez, Jorge; Baldiris-Avila, Rosa; O'byrne-Hoyos, Indira; Kannan, Kurunthachalam

    2006-01-01

    Perfluorinated compounds are widespread pollutants of toxicological importance that have been detected in environmental matrices. However, little is known on their distribution in South America. In this study, distribution of perfluorooctanesulfonate (PFOS), perfluorooctanoic acid (PFOA), perfluorohexanesulfonate (PFHxS), and perfluorooctanesulfonamide (PFOSA) was determined in the bile of mullet, Mugil incilis, and in tissues of pelicans (Pelecanus occidentalis) collected from North Colombia. Analysis was performed by HPLC mass spectrometry after ion-pair extraction. PFOS was found in all bile samples and PFOA and PFHxS were detected at lower frequency. Average concentrations of PFOS, PFOA, and PFHxS in bile of fish from Cartagena Bay, an industrialized site, and Totumo marsh, a reference site, were 3673, 370, 489 and 713, 47.4, 1.27 ng/mL, respectively. PFOS concentrations in pelican organs decreased in the order of spleen > liver > lung > kidney > brain > heart > muscle. These results suggest, for the first time, that perfluorinated compounds are also found in wildlife from Latin American countries. - Perfluorooctanesulfonate and related perfluorinated compounds have been found in a tropical ecosystem of South America

  16. Determination of Coenzyme A and Acetyl-Coenzyme A in Biological Samples Using HPLC with UV Detection

    Directory of Open Access Journals (Sweden)

    Yevgeniya I. Shurubor

    2017-08-01

    Full Text Available Coenzyme A (CoA and acetyl-coenzyme A (acetyl-CoA play essential roles in cell energy metabolism. Dysregulation of the biosynthesis and functioning of both compounds may contribute to various pathological conditions. We describe here a simple and sensitive HPLC-UV based method for simultaneous determination of CoA and acetyl-CoA in a variety of biological samples, including cells in culture, mouse cortex, and rat plasma, liver, kidney, and brain tissues. The limits of detection for CoA and acetyl-CoA are >10-fold lower than those obtained by previously described HPLC procedures, with coefficients of variation <1% for standard solutions, and 1–3% for deproteinized biological samples. Recovery is 95–97% for liver extracts spiked with Co-A and acetyl-CoA. Many factors may influence the tissue concentrations of CoA and acetyl-CoA (e.g., age, fed, or fasted state. Nevertheless, the values obtained by the present HPLC method for the concentration of CoA and acetyl-CoA in selected rodent tissues are in reasonable agreement with literature values. The concentrations of CoA and acetyl-CoA were found to be very low in rat plasma, but easily measurable by the present HPLC method. The method should be useful for studying cellular energy metabolism under normal and pathological conditions, and during targeted drug therapy treatment.

  17. Use of Complementary Approaches to Imaging Biomolecules and Endogenous and Exogenous Trace Elements and Nanoparticles in Biological Samples

    Science.gov (United States)

    Brown, Koshonna Dinettia

    X-ray Fluorescence Microscopy (XFM) is a useful technique for study of biological samples. XFM was used to map and quantify endogenous biological elements as well as exogenous materials in biological samples, such as the distribution of titanium dioxide (TiO2) nanoparticles. TiO 2 nanoparticles are produced for many different purposes, including development of therapeutic and diagnostic particles for cancer detection and treatment, drug delivery, and induction of DNA breaks. Delivery of such nanoparticles can be targeted to specific cells and subcellular structures. In this work, we develop two novel approaches to stain TiO2 nanoparticles for optical microscopy and to confirm that staining by XFM. The first approach utilizes fluorescent biotin and fluorescent streptavidin to label the nanoparticles before and after cellular uptake; the second approach is based on the copper-catalyzed azide-alkyne cycloaddition, the so-called CLICK chemistry, for labeling of azide conjugated TiO2 nanoparticles with "clickable" dyes such as alkyne Alexa Fluor dyes with a high fluorescent yield. To confirm that the optical fluorescence signals of nanoparticles stained in situ match the distribution of the Ti element, we used high resolution synchrotron X-Ray Fluorescence Microscopy (XFM) using the Bionanoprobe instrument at the Advanced Photon Source at Argonne National Laboratory. Titanium-specific X-ray fluorescence showed excellent overlap with the location of Alexa Fluor optical fluorescence detected by confocal microscopy. In this work XFM was also used to investigate native elemental differences between two different types of head and neck cancer, one associated with human papilloma virus infection, the other virus free. Future work may see a cross between these themes, for example, exploration of TiO2 nanoparticles as anticancer treatment for these two different types of head and neck cancer.

  18. On-line preconcentration and determination of mercury in biological and environmental samples by cold vapor-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Ferrua, N.; Cerutti, S.; Salonia, J.A.; Olsina, R.A.; Martinez, L.D.

    2007-01-01

    An on-line procedure for the determination of traces of total mercury in environmental and biological samples is described. The present methodology combines cold vapor generation associated to atomic absorption spectrometry (CV-AAS) with preconcentration of the analyte on a minicolumn packed with activated carbon. The retained analyte was quantitatively eluted from the minicolumn with nitric acid. After that, volatile specie of mercury was generated by merging the acidified sample and sodium tetrahydroborate(III) in a continuous flow system. The gaseous analyte was subsequently introduced via a stream of Ar carrier into the atomizer device. Optimizations of both, preconcentration and mercury volatile specie generation variables were carried out using two level full factorial design (2 3 ) with 3 replicates of the central point. Considering a sample consumption of 25 mL, an enrichment factor of 13-fold was obtained. The detection limit (3σ) was 10 ng L -1 and the precision (relative standard deviation) was 3.1% (n = 10) at the 5 μg L -1 level. The calibration curve using the preconcentration system for mercury was linear with a correlation coefficient of 0.9995 at levels near the detection limit up to at least 1000 μg L -1 . Satisfactory results were obtained for the analysis of mercury in tap water and hair samples

  19. On-line Determination of Zinc in Water and Biological Samples after Its Preconcentration onto Zincon Anchored Polyurethane Foam.

    Science.gov (United States)

    Azeem, Sami M Abdel; Hanafi, Hassan A; El-Shahat, M F

    2015-01-01

    A fast and sensitive on-line procedure for the determination of zinc in water and biological samples was developed. Zinc was preconcentrated in a mini-column packed with polyurethane foam (PUF) chemically modified with zincon via -N=N- bonding. The optimal conditions for preconcentration were pH 8.5 and sample flow rate of 4.0 mL min(-1). Quantitative desorption of Zn(II) was obtained by 0.1 mol L(-1) hydrochloric acid and subsequent spectrophotmetric determination using 4-(2-pyridylazo)-resorcinol at 498 nm. The obtained detection limit was found to be 3.0 ng mL(-1), precision (RSD) was 4.8 and 6.7% at 20 and 110 ng mL(-1), respectively, for 60 s preconcentration time and enrichment factor was 31. The linearity range was from 10 to 120 ng mL(-1) and maximum sample throughput was 20 h(-1). Finally, the method was successfully applied to the determination of zinc in tap water, Nile River water and human urine samples with RSD in the range of 1.1 - 8.3%.

  20. K1-95-HW, cruise report 1995: preliminary results. Phase III: sediment chemistry and biological sampling survey

    Science.gov (United States)

    Torresan, M.E.; Hampton, M.A.; Barber, J.H.; Wong, F.L.

    1995-01-01

    Mamala Bay, off the south shore of the island of Oahu, has been used as a repository of dredged material primarily from Pearl and Honolulu Harbors for over a century. The U.S. Geological Survey, U.S. Army Corps of Engineers, and the U.S. Environmental Protection Agency are conducting an integrated study on the distribution and character of dredged materials as well as the effects of dredged material on the marine environment. A three phase study is providing information to evaluate the effects on seafloor substrate and the benthic fauna. The studies include geophysical profiling and imaging, bottom photography, sampling, chemical and physical analyses of sediment, and evaluations of the benthic population, population density, and adverse impacts to the benthic fauna. Phase 1, conducted in 1993, inventoried the seafloor via remote sensing. Sidescan sonar and subbottom profilers characterized the seafloor in and around the disposal sites, and the resulting products reveal the character and extent of the dredged material. These data were used to plan Phase 2 in 1994, a sampling program that employed subbottom profilers, video and still photography, and seafloor sampling to ground truth the sonar mosaic and identify the seafloor substrates responsible for the various acoustic signatures on the sonar images and subbottom profiles. Box coring provided the samples necessary to distinguish dredged material from native sediment, and for the chemical analyses used to determine contaminant concentrations. Phase 3 studies conducted in June of 1995 consisted of box core sampling for chemical and biological analyses. Specific studies include: infaunal taxonomy and population density, bioassay/bioaccumulation, sediment chemistry, and post-disposal resuspension and transport. The 1995 survey, conducted June 14 through 17, resulted in the collection of 39 box cores from 20 different stations. Multiple box cores were composited at 7 different locations occupied in 1994, to provide

  1. Gay and Bisexual Men's Perceptions of the Donation and Use of Human Biological Samples for Research: A Qualitative Study.

    Directory of Open Access Journals (Sweden)

    Chris Patterson

    Full Text Available Human biological samples (biosamples are increasingly important in diagnosing, treating and measuring the prevalence of illnesses. For the gay and bisexual population, biosample research is particularly important for measuring the prevalence of human immunodeficiency virus (HIV. By determining people's understandings of, and attitudes towards, the donation and use of biosamples, researchers can design studies to maximise acceptability and participation. In this study we examine gay and bisexual men's attitudes towards donating biosamples for HIV research. Semi-structured telephone interviews were conducted with 46 gay and bisexual men aged between 18 and 63 recruited in commercial gay scene venues in two Scottish cities. Interview transcripts were analysed thematically using the framework approach. Most men interviewed seemed to have given little prior consideration to the issues. Participants were largely supportive of donating tissue for medical research purposes, and often favourable towards samples being stored, reused and shared. Support was often conditional, with common concerns related to: informed consent; the protection of anonymity and confidentiality; the right to withdraw from research; and ownership of samples. Many participants were in favour of the storage and reuse of samples, but expressed concerns related to data security and potential misuse of samples, particularly by commercial organisations. The sensitivity of tissue collection varied between tissue types and collection contexts. Blood, urine, semen and bowel tissue were commonly identified as sensitive, and donating saliva and as unlikely to cause discomfort. To our knowledge, this is the first in-depth study of gay and bisexual men's attitudes towards donating biosamples for HIV research. While most men in this study were supportive of donating tissue for research, some clear areas of concern were identified. We suggest that these minority concerns should be accounted

  2. Subcellular imaging of isotopically labeled carbon compounds in a biological sample by ion microprobe (NanoSIMS).

    Science.gov (United States)

    Clode, Peta L; Stern, Richard A; Marshall, Alan T

    2007-03-01

    Here we demonstrate the technique of nanoscale secondary ion mass spectrometry, utilizing the Cameca NanoSIMS50 ion microprobe, to detect and image the metabolism of an isotopically labeled compound (NaH(13)CO(3)) in a biological sample. In particular, we have designed and verified protocols for imaging the subcellular distribution and determining the relative abundance of labeled (13)C, within the coral Galaxea fascicularis. Analyses were conducted on 1-mum thick sections of resin-embedded material, using both scanned (mapping) and static (spot analysis) Cs(+) primary ion beam of approximately 100 nm diameter. Using these samples we establish that NanoSIMS has adequate mass resolution to reliably distinguish (13)C from potential isobaric interference by (12)C(1)H and that data extracted from ion maps are comparable to those acquired by spot analyses. Independent of the method of acquisition, ratioing of (13)C to the naturally abundant (12)C is essential if meaningful data, which can be statistically compared to standard and control samples, are to be obtained. These results highlight the potential of NanoSIMS for intracellular tracking of a variety of organic and inorganic compounds labeled with stable isotopes of C, N, O, S, P, and halogens. (c) 2007 Wiley-Liss, Inc.

  3. [A novel flow injection chemiluminescence method with ferricyanide and luminol for the determination of ractopamine in biological samples].

    Science.gov (United States)

    Feng, Ting; Hu, Yu-fei; Li, Gong-ke

    2012-01-01

    A novel chemiluminescence method coupled with flow injection technique for the determination of ractopamine was developed. It was based on the enhancement of the chemiluminescence by ractopamine derived from the chemiluminescence reaction between luminol and ferricyanide in sodium hydroxide medium. The linear calibration range of the chemiluminescence intensity with respect to the ractopamine concentration covers from 4.0 x 10(-9) - 8.0 x 10(-7) g x mL(-1). The relative standard deviation for ractopamine is 5.6% (n = 11), and the detection limit is 2.5 x 10(-9) g x mL(-1). The method was firstly applied to the determination of ractopamine in biological samples with satisfactory results. The recovery was between 69.3% and 101.3%.

  4. Highly sensitive and specific analysis of sterol profiles in biological samples by HPLC-ESI-MS/MS.

    Science.gov (United States)

    Honda, Akira; Miyazaki, Teruo; Ikegami, Tadashi; Iwamoto, Junichi; Yamashita, Kouwa; Numazawa, Mitsuteru; Matsuzaki, Yasushi

    2010-08-01

    High-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) is a powerful method for the microanalysis of compounds in biological samples. Compared with gas chromatography-mass spectrometry (GC-MS), this method is more broadly applicable to various compounds and usually does not require a derivatization step before analysis. However, when neutral sterols are analyzed, the sensitivities of usual HPLC-MS/MS method are not superior to those of GC-MS because the sterols are relatively resistant to ionization. In this review, we introduce the recent development of HPLC-MS/MS analysis for the quantification of non-cholesterol sterols. By adding an effective derivatization step to the conventional procedure, sterol analysis by HPLC-MS/MS surpassed that obtained by GC-MS in sensitivity. In addition, sufficient specificity of this method was achieved by selected reaction monitoring (SRM) and thorough chromatographic separation of each sterol. Copyright 2010 Elsevier Ltd. All rights reserved.

  5. Graphene-Based Materials as Solid Phase Extraction Sorbent for Trace Metal Ions, Organic Compounds, and Biological Sample Preparation.

    Science.gov (United States)

    Ibrahim, Wan Aini Wan; Nodeh, Hamid Rashidi; Sanagi, Mohd Marsin

    2016-07-03

    Graphene is a new carbon-based material that is of interest in separation science. Graphene has extraordinary properties including nano size, high surface area, thermal and chemical stability, and excellent adsorption affinity to pollutants. Its adsorption mechanisms are through non-covalent interactions (π-π stacking, electrostatic interactions, and H-bonding) for organic compounds and covalent interactions for metal ions. These properties have led to graphene-based material becoming a desirable adsorbent in a popular sample preparation technique known as solid phase extraction (SPE). Numerous studies have been published on graphene applications in recent years, but few review papers have focused on its applications in analytical chemistry. This article focuses on recent preconcentration of trace elements, organic compounds, and biological species using SPE-based graphene, graphene oxide, and their modified forms. Solid phase microextraction and micro SPE (µSPE) methods based on graphene are discussed.

  6. Recent progress of task-specific ionic liquids in chiral resolution and extraction of biological samples and metal ions.

    Science.gov (United States)

    Wu, Datong; Cai, Pengfei; Zhao, Xiaoyong; Kong, Yong; Pan, Yuanjiang

    2018-01-01

    Ionic liquids have been functionalized for modern applications. The functional ionic liquids are also called task-specific ionic liquids. Various task-specific ionic liquids with certain groups have been constructed and exploited widely in the field of separation. To take advantage of their properties in separation science, task-specific ionic liquids are generally used in techniques such as liquid-liquid extraction, solid-phase extraction, gas chromatography, high-performance liquid chromatography, and capillary electrophoresis. This review mainly covers original research papers published in the last five years, and we will focus on task-specific ionic liquids as the chiral selectors in chiral resolution and as extractant or sensor for biological samples and metal ion purification. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  7. New Detection Modality for Label-Free Quantification of DNA in Biological Samples via Superparamagnetic Bead Aggregation

    Science.gov (United States)

    Leslie, Daniel C.; Li, Jingyi; Strachan, Briony C.; Begley, Matthew R.; Finkler, David; Bazydlo, Lindsay L.; Barker, N. Scott; Haverstick, Doris; Utz, Marcel; Landers, James P.

    2012-01-01

    Combining DNA and superparamagnetic beads in a rotating magnetic field produces multiparticle aggregates that are visually striking, and enables label-free optical detection and quantification of DNA at levels in the picogram per microliter range. DNA in biological samples can be quantified directly by simple analysis of optical images of microfluidic wells placed on a magnetic stirrer without DNA purification. Aggregation results from DNA/bead interactions driven either by the presence of a chaotrope (a nonspecific trigger for aggregation) or by hybridization with oligonucleotides on functionalized beads (sequence-specific). This paper demonstrates quantification of DNA with sensitivity comparable to that of the best currently available fluorometric assays. The robustness and sensitivity of the method enable a wide range of applications, illustrated here by counting eukaryotic cells. Using widely available and inexpensive benchtop hardware, the approach provides a highly accessible low-tech microscale alternative to more expensive DNA detection and cell counting techniques. PMID:22423674

  8. Development of a radiochemical neutron activation analysis procedure for determination of rhenium in biological and environmental samples at ultratrace level

    International Nuclear Information System (INIS)

    Kucera, J.; Lucanikova, M.; Czech Technical Univ., Prague

    2006-01-01

    Radiochemical neutron activation procedures using liquid-liquid extraction with tetraphenylarsonium chloride in chloroform from 1M HCl and solid extraction with ALIQUAT 336 incorporated in a polyacrylonitrile binding matrix from 0.1M HCl were developed for accurate determination of rhenium in biological and environmental samples at the sub-ng x g -1 level. Concentrations of Re in the range of 0.1 to 2.4 ng x g -1 were determined in several botanical reference materials (RM), while in a RM of road dust a value of ∼ 10 ng x g -1 was found. Significantly elevated values of Re, up to 90 ng x g -1 were found in seaweed (brown algae). Results for Re in the brown algae Fucus vesiculosus in which elevated 99 Tc values had previously been determined suggested possible competition between Re and Tc in the accumulation process. (author)

  9. A human monocytic NF-κB fluorescent reporter cell line for detection of microbial contaminants in biological samples.

    Directory of Open Access Journals (Sweden)

    Claire Battin

    Full Text Available Sensing of pathogens by innate immune cells is essential for the initiation of appropriate immune responses. Toll-like receptors (TLRs, which are highly sensitive for various structurally and evolutionary conserved molecules derived from microbes have a prominent role in this process. TLR engagement results in the activation of the transcription factor NF-κB, which induces the expression of cytokines and other inflammatory mediators. The exquisite sensitivity of TLR signalling can be exploited for the detection of bacteria and microbial contaminants in tissue cultures and in protein preparations. Here we describe a cellular reporter system for the detection of TLR ligands in biological samples. The well-characterized human monocytic THP-1 cell line was chosen as host for an NF-ᴋB-inducible enhanced green fluorescent protein reporter gene. We studied the sensitivity of the resultant reporter cells for a variety of microbial components and observed a strong reactivity towards TLR1/2 and TLR2/6 ligands. Mycoplasma lipoproteins are potent TLR2/6 agonists and we demonstrate that our reporter cells can be used as reliable and robust detection system for mycoplasma contaminations in cell cultures. In addition, a TLR4-sensitive subline of our reporters was engineered, and probed with recombinant proteins expressed in different host systems. Bacterially expressed but not mammalian expressed proteins induced strong reporter activity. We also tested proteins expressed in an E. coli strain engineered to lack TLR4 agonists. Such preparations also induced reporter activation in THP-1 cells highlighting the importance of testing recombinant protein preparations for microbial contaminations beyond endotoxins. Our results demonstrate the usefulness of monocytic reporter cells for high-throughput screening for microbial contaminations in diverse biological samples, including tissue culture supernatants and recombinant protein preparations. Fluorescent reporter

  10. An exploratory study of red raspberry (Rubus idaeus L.) (poly)phenols/metabolites in human biological samples.

    Science.gov (United States)

    Zhang, Xuhuiqun; Sandhu, Amandeep; Edirisinghe, Indika; Burton-Freeman, Britt

    2018-02-21

    Red raspberry (Rubus idaeus L.) contains a variety of polyphenols including anthocyanins and ellagitannins. Red raspberry polyphenols absorbed in different forms (parent compounds, degradants or microbial metabolites) are subject to xenobiotic metabolism in the intestine, liver, and/or kidney, forming methylate, glucuronide, and sulfate conjugated metabolites. Upon acute exposure, (poly)phenol/metabolite presence in the blood depends mainly on intestinal absorption, enterohepatic circulation, and metabolism by resident microbiota. However, chronic exposure to red raspberry polyphenols may alter metabolite patterns depending on adaptions in the xenobiotic machinery and/or microbiota composition. Understanding the metabolic fate of these compounds and their composition in different biological specimens relative to the exposure time/dose will aid in designing future health benefit studies, including the mechanism of action studies. The present exploratory study applied ultra-high performance liquid chromatography (UHPLC) coupled with quadrupole time-of-flight (QTOF) and triple quadrupole (QQQ) mass spectrometries to characterize red raspberry polyphenols in fruit and then their appearance, including metabolites in human biological samples (plasma, urine and breast milk) after the chronic intake of red raspberries. The results suggested that the most abundant polyphenols in red raspberries included cyanidin 3-O-sophoroside, cyanidin 3-O-glucoside, sanguiin H6 and lambertianin C. Sixty-two (poly)phenolic compounds were tentatively identified in the plasma, urine and breast milk samples after the intake of red raspberries. In general, urine contained the highest content of phenolic metabolites; phase II metabolites, particularly sulfated conjugates, were mainly present in urine and breast milk, and breast milk contained fewer parent anthocyanins compared to urine and plasma.

  11. Evaluation of calcium, magnesium, potassium, and sodium in biological samples (scalp hair, serum, blood, and urine) of Pakistani referents and arthritis patients of different age groups.

    Science.gov (United States)

    Afridi, Hassan Imran; Kazi, Tasneem Gul; Kazi, Naveed; Shah, Abdul Qadir; Khan, Sumaira; Kolachi, Nida Fatima; Wadhwa, Sham Kumar; Shah, Faheem

    2012-01-01

    Rheumatoid Arthritis is a chronic inflammatory disease resulting in joint inflammation (particularly joints of hands, wrists, feet, knees, ankles, and shoulder) that is manifested by swelling and functional impairment. This study was designed to compare the levels of calcium (Ca), magnesium (mg), potassium (K), and sodium (Na) in four biological samples (scalp hair, serum, blood, and urine) of patients with rheumatoid arthritis (RA) as compared to referent subjects of both genders who do have not arthritis problems. All patients and referents were divided in two age groups, (46-60) and (61-75) years. A microwave assisted wet acid digestion procedure was used for acid digestion of biological samples. The digests of all biological samples were analysed for Ca, Mg, K, and Na by flame atomic absorption spectrometry (FAAS). The proposed method was validated by using conventional wet digestion of the same sub samples and certified reference samples of hair, serum, blood, and urine. The results indicated significantly lower levels of Ca, Mg, and K in the biological samples (blood, serum, and scalp hair) of male and female rheumatoid arthritis patients when compared to referents of both genders, whereas the levels of Na were found to be high in blood and urine samples of patients as compared to nonrheumatic referents. These data represent a guide for clinicians and other professionals who will be investigating the deficiency of essential micronutrients in biological samples (scalp hair, serum, and blood) of rheumatoid arthritis patients.

  12. Determination of As, Cd, Cu, Hg and Pb in biological samples by modern electrothermal atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Sardans, Jordi, E-mail: j.sardans@creaf.uab.ca [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain); Montes, Fernando [Departamento de Ciencias Analiticas, Facultad de Ciencias, Universidad Nacional de Educacion a Distancia (UNED), C/ Senda del Rey 9. 28040 Madrid (Spain); Penuelas, Josep [Ecophysiological and Global Change Unit CSIC-CREAF, Edifici C, Universitat Autonoma de Barcelona, Bellaterra 08193, Barcelona (Spain)

    2010-02-15

    of this technique that reaches figures of merit equivalent to Inductively coupled plasma mass spectrometry (ICP-MS). Herein is presented an overview of recent advances and applications of (ETAAS) for the determination of As, Cd, Cu, Hg and Pb in biological samples drawn from studies over the last decade.

  13. Evaluation of non-invasive biological samples to monitor Staphylococcus aureus colonization in great apes and lemurs.

    Directory of Open Access Journals (Sweden)

    Frieder Schaumburg

    Full Text Available Reintroduction of endangered animals as part of conservational programs bears the risk of importing human pathogens from the sanctuary to the natural habitat. One bacterial pathogen that serves as a model organism to analyze this transmission is Staphylococcus aureus as it can colonize and infect both humans and animals. The aim of this study was to evaluate the utility of various biological samples to monitor S. aureus colonization in great apes and lemurs.Mucosal swabs from wild lemurs (n=25, Kirindy, Madagascar, feces, oral and genital swabs from captive chimpanzees (n=58, Ngamba and Entebbe, Uganda and fruit wadges and feces from wild chimpanzees (n=21, Taï National Parc, Côte d'Ivoire were screened for S. aureus. Antimicrobial resistance and selected virulence factors were tested for each isolate. Sequence based genotyping (spa typing, multilocus sequence typing was applied to assess the population structure of S. aureus.Oro-pharyngeal carriage of S. aureus was high in lemurs (72%, n=18 and captive chimpanzees (69.2%, n=27 and 100%, n=6, respectively. Wild chimpanzees shed S. aureus through feces (43.8, n=7 and fruit wadges (54.5, n=12. Analysis of multiple sampling revealed that two samples are sufficient to detect those animals which shed S. aureus through feces or fruit wadges. Genotyping showed that captive animals are more frequently colonized with human-associated S. aureus lineages.Oro-pharyngeal swabs are useful to screen for S. aureus colonization in apes and lemurs before reintroduction. Duplicates of stool and fruit wadges reliably detect S. aureus shedding in wild chimpanzees. We propose to apply these sampling strategies in future reintroduction programs to screen for S. aureus colonization. They may also be useful to monitor S. aureus in wild populations.

  14. X-ray holographic microscopy with zone plates applied to biological samples in the water window using 3rd harmonic radiation from the free-electron laser FLASH.

    Science.gov (United States)

    Gorniak, T; Heine, R; Mancuso, A P; Staier, F; Christophis, C; Pettitt, M E; Sakdinawat, A; Treusch, R; Guerassimova, N; Feldhaus, J; Gutt, C; Grübel, G; Eisebitt, S; Beyer, A; Gölzhäuser, A; Weckert, E; Grunze, M; Vartanyants, I A; Rosenhahn, A

    2011-06-06

    The imaging of hydrated biological samples - especially in the energy window of 284-540 eV, where water does not obscure the signal of soft organic matter and biologically relevant elements - is of tremendous interest for life sciences. Free-electron lasers can provide highly intense and coherent pulses, which allow single pulse imaging to overcome resolution limits set by radiation damage. One current challenge is to match both the desired energy and the intensity of the light source. We present the first images of dehydrated biological material acquired with 3rd harmonic radiation from FLASH by digital in-line zone plate holography as one step towards the vision of imaging hydrated biological material with photons in the water window. We also demonstrate the first application of ultrathin molecular sheets as suitable substrates for future free-electron laser experiments with biological samples in the form of a rat fibroblast cell and marine biofouling bacteria Cobetia marina.

  15. A tree-like Bayesian structure learning algorithm for small-sample datasets from complex biological model systems.

    Science.gov (United States)

    Yin, Weiwei; Garimalla, Swetha; Moreno, Alberto; Galinski, Mary R; Styczynski, Mark P

    2015-08-28

    There are increasing efforts to bring high-throughput systems biology techniques to bear on complex animal model systems, often with a goal of learning about underlying regulatory network structures (e.g., gene regulatory networks). However, complex animal model systems typically have significant limitations on cohort sizes, number of samples, and the ability to perform follow-up and validation experiments. These constraints are particularly problematic for many current network learning approaches, which require large numbers of samples and may predict many more regulatory relationships than actually exist. Here, we test the idea that by leveraging the accuracy and efficiency of classifiers, we can construct high-quality networks that capture important interactions between variables in datasets with few samples. We start from a previously-developed tree-like Bayesian classifier and generalize its network learning approach to allow for arbitrary depth and complexity of tree-like networks. Using four diverse sample networks, we demonstrate that this approach performs consistently better at low sample sizes than the Sparse Candidate Algorithm, a representative approach for comparison because it is known to generate Bayesian networks with high positive predictive value. We develop and demonstrate a resampling-based approach to enable the identification of a viable root for the learned tree-like network, important for cases where the root of a network is not known a priori. We also develop and demonstrate an integrated resampling-based approach to the reduction of variable space for the learning of the network. Finally, we demonstrate the utility of this approach via the analysis of a transcriptional dataset of a malaria challenge in a non-human primate model system, Macaca mulatta, suggesting the potential to capture indicators of the earliest stages of cellular differentiation during leukopoiesis. We demonstrate that by starting from effective and efficient approaches

  16. Towards a system level understanding of non-model organisms sampled from the environment: a network biology approach.

    Directory of Open Access Journals (Sweden)

    Tim D Williams

    2011-08-01

    Full Text Available The acquisition and analysis of datasets including multi-level omics and physiology from non-model species, sampled from field populations, is a formidable challenge, which so far has prevented the application of systems biology approaches. If successful, these could contribute enormously to improving our understanding of how populations of living organisms adapt to environmental stressors relating to, for example, pollution and climate. Here we describe the first application of a network inference approach integrating transcriptional, metabolic and phenotypic information representative of wild populations of the European flounder fish, sampled at seven estuarine locations in northern Europe with different degrees and profiles of chemical contaminants. We identified network modules, whose activity was predictive of environmental exposure and represented a link between molecular and morphometric indices. These sub-networks represented both known and candidate novel adverse outcome pathways representative of several aspects of human liver pathophysiology such as liver hyperplasia, fibrosis, and hepatocellular carcinoma. At the molecular level these pathways were linked to TNF alpha, TGF beta, PDGF, AGT and VEGF signalling. More generally, this pioneering study has important implications as it can be applied to model molecular mechanisms of compensatory adaptation to a wide range of scenarios in wild populations.

  17. High-resolution, high-transmission soft x-ray spectrometer for the study of biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Fuchs, O.; Weinhardt, L.; Blum, M.; Weigand, M.; Umbach, E. [Universitaet Wuerzburg, Experimentelle Physik II, Am Hubland, 97074 Wuerzburg (Germany); Baer, M.; Heske, C. [Department of Chemistry, University of Nevada, 4505 Maryland Pkwy., Las Vegas, Nevada 89154-4003 (United States); Denlinger, J.; Chuang, Y.-D.; McKinney, W.; Hussain, Z. [Advanced Light Source, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); Gullikson, E.; Jones, M.; Batson, P. [Center for X-Ray Optics, Material Science Division, Lawrence Berkeley National Laboratory, Berkeley, California 94720 (United States); Nelles, B. [Carl Zeiss Laser Optics GmbH, Carl-Zeiss-Str. 22, 73447 Oberkochen (Germany); Follath, R. [Berliner Elektronenspeicherring-Gesellschaft fuer Synchrotronstrahlung m.b.H., Albert-Einstein-Str. 15, 12489 Berlin (Germany)

    2009-06-15

    We present a variable line-space grating spectrometer for soft x-rays that covers the photon energy range between 130 and 650 eV. The optical design is based on the Hettrick-Underwood principle and tailored to synchrotron-based studies of radiation-sensitive biological samples. The spectrometer is able to record the entire spectral range in one shot, i.e., without any mechanical motion, at a resolving power of 1200 or better. Despite its slitless design, such a resolving power can be achieved for a source spot as large as (30x3000) {mu}m{sup 2}, which is important for keeping beam damage effects in radiation-sensitive samples low. The high spectrometer efficiency allows recording of comprehensive two-dimensional resonant inelastic soft x-ray scattering (RIXS) maps with good statistics within several minutes. This is exemplarily demonstrated for a RIXS map of highly oriented pyrolytic graphite, which was taken within 10 min.

  18. Sensitive determination of fluoride in biological samples by gas chromatography-mass spectrometry after derivatization with 2-(bromomethyl)naphthalene.

    Science.gov (United States)

    Kwon, Sun-Myung; Shin, Ho-Sang

    2014-12-10

    A gas chromatography-mass spectrometric method was developed in this study in order to determine fluoride in plasma and urine after derivatization with 2-(bromomethyl)naphthalene. 2-Fluoronaphthalene was chosen as the internal standard. The derivatization of fluoride was performed in the biological sample and the best reaction conditions (10.0 mg mL(-1) of 2-(bromomethyl)naphthalene, 1.0 mg mL(-1) of 15-crown-5-ether as a phase transfer catalyst, pH of 7.0, reaction temperature of 70°C, and heating time of 70 min) were established. The organic derivative was extracted with dichloromethane and then measured by a gas chromatography-mass spectrometry. Under the established condition, the detection limits were 11 μg L(-1) and 7 μg L(-1) by using 0.2 mL of plasma or urine, respectively. The accuracy was in a range of 100.8-107.6%, and the precision of the assay was less than 4.3% in plasma or urine. Fluoride was detected in a concentration range of 0.12-0.53 mg L(-1) in six urine samples after intake of natural mineral water containing 0.7 mg L(-1) of fluoride. Copyright © 2014 Elsevier B.V. All rights reserved.

  19. The IAEA worldwide intercomparison exercises (1990-1997). Determination of trace elements in marine sediments and biological samples

    International Nuclear Information System (INIS)

    Coquery, M.; Carvalho, F.P.; Azemard, S.; Horvat, M.

    1999-01-01

    Four major worldwide intercomparison exercises for the determination of trace elements in various environmental matrices were completed by the IAEA Marine Environment Laboratory since 1990: SD-M-2/TM, deep sea marine sediment; IAEA-350, tuna fish homogenate; IAEA-356, contaminated coastal sediment and IAEA-140, sea plant (Fucus sp.). These intercomparison exercises aim at enabling individual laboratories to monitor their performance. The results of these exercises allowed us to make an overall evaluation of the quality of data provided for environmental assessment and to identify the trends of analytical performance in the determination of trace elements over the years. The number of participants in each exercise varied between 68 and 130, and permits statistical evaluation of the performance for a number of elements. For each intercomparison exercise, the performance of the participant laboratories was assessed by comparing reported results with established reference values calculating 'Z-scores'. The results show that for each sample matrix, the values reported by some laboratories were far from satisfactory in the earlier exercises, in particular for Cd, Cr and Pb. Nevertheless, over time, a general improvement of performance can clearly be seen for all elements. Moreover, there was a noticeable increase in the number of laboratories with good performance in the two most recent exercises, observed both for biological and for sediment matrices. However, the determination of trace elements such as Cd, Cr, Pb and Hg in low level environmental samples still remains a major challenge to the analysts. For this reason and in order to assess the current performance of laboratories for low environmental levels of contaminants, the future intercomparison exercises will concentrate on low level sediment and fish samples

  20. Mercury in Environmental and Biological Samples Using Online Combustion with Sequential Atomic Absorption and Fluorescence Measurements: A Direct Comparison of Two Fundamental Techniques in Spectrometry

    Science.gov (United States)

    Cizdziel, James V.

    2011-01-01

    In this laboratory experiment, students quantitatively determine the concentration of an element (mercury) in an environmental or biological sample while comparing and contrasting the fundamental techniques of atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). A mercury analyzer based on sample combustion,…

  1. Preliminary biological sampling of GT3 and BT1 cores and the microbial community dynamics of existing subsurface wells

    Science.gov (United States)

    Kraus, E. A.; Stamps, B. W.; Rempfert, K. R.; Ellison, E. T.; Nothaft, D. B.; Boyd, E. S.; Templeton, A. S.; Spear, J. R.

    2017-12-01

    Subsurface microbial life is poorly understood but potentially very important to the search for life on other planets as well as increasing our understanding of Earth's geobiological processes. Fluids and rocks of actively serpentinizing subsurface environments are a recent target of biological study due to their apparent ubiquity across the solar system. Areas of serpentinization can contain high concentrations of molecular hydrogen, H2, that can serve as the dominant fuel source for subsurface microbiota. Working with the Oman Drilling Project, DNA and RNA were extracted from fluids of seven alkaline wells and two rock cores from drill sites GT3 and BT1 within the Samail ophiolite. DNA and cDNA (produced via reverse transcription from the recovered RNA) were sequenced using universal primers to identify microbial life across all three domains. Alkaline subsurface fluids support a microbial community that changes with pH and host-rock type. In peridotite with pH values of >11, wells NSHQ 14 and WAB 71 have high relative abundances of Meiothermus, Methanobacterium, the family Nitrospiraceae, and multiple types of the class Dehalococcoidia. While also hosted in peridotite but at pH 8.5, wells WAB 104 and 105 have a distinct, more diverse microbial community. This increased variance in community make-up is seen in wells that sit near/at the contact of gabbro and peridotite formations as well. Core results indicate both sampled rock types host a very low biomass environment subject to multiple sources of contamination during the drilling process. Suggestions for contaminant reduction, such as having core handlers wear nitrile gloves and flame-sterilizing the outer surfaces of core rounds for biological sampling, would have minimal impact to overall ODP coreflow and maximize the ability to better understand in situ microbiota in this low-biomass serpentinizing subsurface environment. While DNA extraction was successful with gram amounts of crushed rock, much can be

  2. HPLC and TLC methods for analysis of [18F]FDG and its metabolites from biological samples.

    Science.gov (United States)

    Rokka, Johanna; Grönroos, Tove J; Viljanen, Tapio; Solin, Olof; Haaparanta-Solin, Merja

    2017-03-24

    The most used positron emission tomography (PET) tracer, 2-[ 18 F]fluoro-2-deoxy-d-glucose ([ 18 F]FDG), is a glucose analogue that is used to measure tissue glucose consumption. Traditionally, the Sokoloff model is the basis for [ 18 F]FDG modeling. According to this model, [ 18 F]FDG is expected to be trapped in a cell in the form of [ 18 F]FDG-6-phosphate ([ 18 F]FDG-6-P). However, several studies have shown that in tissues, [ 18 F]FDG metabolism goes beyond [ 18 F]FDG-6-P. Our aim was to develop radioHPLC and radioTLC methods for analysis of [ 18 F]FDG metabolites from tissue samples. The radioHPLC method uses a sensitive on-line scintillation detector to detect radioactivity, and the radioTLC method employs digital autoradiography to detect the radioactivity distribution on a TLC plate. The HPLC and TLC methods were developed using enzymatically in vitro-produced metabolites of [ 18 F]FDG as reference standards. For this purpose, three [ 18 F]FDG metabolites were synthesized: [ 18 F]FDG-6-P, [ 18 F]FD-PGL, and [ 18 F]FDG-1,6-P2. The two methods were evaluated by analyzing the [ 18 F]FDG metabolic profile from rodent ex vivo tissue homogenates. The HPLC method with an on-line scintillation detector had a wide linearity in a range of 5Bq-5kBq (LOD 46Bq, LOQ 139Bq) and a good resolution (Rs ≥1.9), and separated [ 18 F]FDG and its metabolites clearly. The TLC method combined with digital autoradiography had a high sensitivity in a wide range of radioactivity (0.1Bq-2kBq, LOD 0.24Bq, LOQ 0.31Bq), and multiple samples could be analyzed simultaneously. As our test and the method validation with ex vivo samples showed, both methods are useful, and at best they complement each other in analysis of [ 18 F]FDG and its radioactive metabolites from biological samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Sample preparation of biological macromolecular assemblies for the determination of high-resolution structures by cryo-electron microscopy.

    Science.gov (United States)

    Stark, Holger; Chari, Ashwin

    2016-02-01

    Single particle cryo-EM has recently developed into a powerful tool to determine the 3D structure of macromolecular complexes at near-atomic resolution, which allows structural biologists to build atomic models of proteins. All technical aspects of cryo-EM technology have been considerably improved over the last two decades, including electron microscopic hardware, image processing software and the ever growing speed of computers. This leads to a more widespread use of the technique, and it can be anticipated that further automation of electron microscopes and image processing tools will soon fully shift the focus away from the technological aspects, onto biological questions that can be answered. In single particle cryo-EM, no crystals of a macromolecule are required. In contrast to X-ray crystallography, this significantly facilitates structure determination by cryo-EM. Nevertheless, a relatively high level of biochemical control is still essential to obtain high-resolution structures by cryo-EM, and it can be anticipated that the success of the cryo-EM technology goes hand in hand with further developments of sample purification and preparation techniques. This will allow routine high-resolution structure determination of the many macromolecular complexes of the cell that until now represent evasive targets for X-ray crystallographers. Here we discuss the various biochemical tools that are currently available and the existing sample purification and preparation techniques for cryo-EM grid preparation that are needed to obtain high-resolution images for structure determination. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  4. [Sensitive determination of reactive oxygen species by chemiluminescence methods and their application to biological samples and health foods].

    Science.gov (United States)

    Wada, Mitsuhiro

    2008-07-01

    Sensitive and selective methods, based on chemiluminescence reactions, were introduced for determination of reactive oxygen species (ROS) and their applications to biological samples and health foods. First, a sensitive method for determination of H(2)O(2) by peroxyoxalate chemiluminescence (PO-CL) was developed. This method could be applied to determine small amounts of H(2)O(2) in cola drinks and bacterial contamination of food items. Secondly, the combination of immobilized enzyme column reactor, or ultraviolet irradiation system, with the PO-CL detection method was able to determine clinical substrates (i.e. choline-containing phospholipids, polyamines and D-amino acids) and organic peroxides. Also, an evaluation method of the quenching effect of luminol chemiluminescence against ROS was developed. The sensitive, rapid and precise measurement of the quenching effect against ROS such as superoxide, singlet oxygen, hydroxyl radical, peroxynitrite and hypochlorous ion was achieved. The proposed method could be applied to rosemary extracts, natural colorants and grape seed extracts.

  5. Spectrofluorimetric determination of buparvaquone in biological fluids, food samples and a pharmaceutical formulation by using terbium-deferasirox probe.

    Science.gov (United States)

    Manzoori, Jamshid L; Jouyban, Abolghasem; Amjadi, Mohammad; Panahi-Azar, Vahid; Karami-Bonari, Amir Reza; Tamizi, Elnaz

    2011-06-15

    A simple spectrofluorimetric method is described for the determination of buparvaquone (BPQ), based on its quenching effect on the fluorescence intensity of Tb(3+)-deferasirox (DFX) complex as a fluorescent probe. The excitation and emission wavelengths were 328 and 545nm, respectively. The optimum conditions for determination of BPQ were investigated considering the effects of various affecting parameters. The variations in fluorescence intensity of the system showed a good linear relationship with the concentration of BPQ in the range of 10-1500μgL(-1), its correlation coefficient was 0.999 with the detection and quantification limits of 1.1 and 3.4μgL(-1), respectively. Linearity, reproducibility, recovery, limits of detection and quantification made the method suitable for BPQ assay in biological fluids, meat, dairy products and BPQ parenteral solutions (vials). The method was applied to real samples of serum and milk of three cows receiving BPQ. Copyright © 2010 Elsevier Ltd. All rights reserved.

  6. Selective solid-phase extraction of cholesterol using molecularly imprinted polymers and its application in different biological samples.

    Science.gov (United States)

    Shi, Yun; Zhang, Jiang-Hua; Shi, Dan; Jiang, Ming; Zhu, Ye-Xiang; Mei, Su-Rong; Zhou, Yi-Kai; Dai, Kang; Lu, Bin

    2006-11-16

    Non-covalent molecularly imprinted polymers (MIPs) of cholesterol were prepared by UV initiated polymerization. A polymer that had the highest binding selectivity and capability was used as solid-phase extraction (SPE) sorbents for direct extraction of cholesterol from different biological samples (human serum, cow milk, yolk, shrimp, pork and beef). The extraction conditions of molecularly imprinted SPE (MISPE) were optimized and the optimum protocol was: conditioning MISPE cartridges with n-hexane, loading with n-hexane, washing with n-hexane and n-hexane:toluene=9:1, respectively, then eluting with chloroform:ethanol:acetic acid=3:1:1. Cholesterol MISPE selectively recognized, effectively trapped and pre-concentrated cholesterol over a concentration range of 10-80 microg/mL. Recoveries ranged from 80.6% to 92.7%, with R.S.D. lower than 9.8%. Under the optimal condition, MISPE recoveries of spiked human serum, yolk, cow milk, shrimp, pork and beef were 91.1%, 80.4%, 86.6%, 78.2%, 81.4% and 80.1%, respectively. Compared with C18 SPE, almost all of the matrix interferences were removed after MISPE, and better baselines and higher selectivity were achieved.

  7. Analysis of inorganic elements in biological samples of C57BL/6J mouse strain using INAA

    International Nuclear Information System (INIS)

    Metairon, Sabrina; Zamboni, Cibele B.; Suzuki, Miriam F.; Kovacs, Luciana; Bueno Junior, Carlos R.

    2013-01-01

    The research for new medicine, vaccines and other products of interest in health area, for any disease, requires several in vivo tests using animal models on experiments for clinical analysis of actions in organism, focusing on the relation between these and the responses or reactions to their use, allowing or not their use in human being. The present investigation deals with the determination of elements concentration (Ca, Cl, K, Mg and Na) of clinical relevance in kidney and liver of C57BL/6J mice strain using the Instrumental Neutron Activation Analysis technique. Particularly, the C57BL/6J strain is one of the most widely used mice genetically modified for human disease studies. The biological samples were collected from 2 month old adult mice bred in the Biotherium (animal breeding) of UNIFESP (Federal University of Sao Paulo, Brasil) and at Human Genome Research Center (University of Sao Paulo, Brasil) and Biotechnology Center (IPEN, Sao Paulo, Brasil). The measurements were performed in the nuclear reactor IEA-R1 (3.5-4.5MW, pool type) at IPEN. These data will allow researchers to optimize their studies, both in terms of cost and time, by knowing the basal reference values in blood and organs of this strain. Additionally, this analytical procedure meets the needs of the world tendency that emphasizes the requirements to propose alternative methods for clinical research that contribute to animal welfare. (author)

  8. Analysis of inorganic elements in biological samples of C57BL/6J mouse strain using INAA

    Energy Technology Data Exchange (ETDEWEB)

    Metairon, Sabrina; Zamboni, Cibele B.; Suzuki, Miriam F.; Kovacs, Luciana, E-mail: metairon@usp.br, E-mail: czamboni@ipen.br, E-mail: mfsuzuki@ipen.br, E-mail: lukovacs@gmail.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Bueno Junior, Carlos R., E-mail: carmao11@yahoo.com.br [Universidade de Sao Paulo (IB/USP), Sao Paulo, SP (Brazil). Instituto de Biociencias. Centro de Estudos do Genoma Humano

    2013-07-01

    The research for new medicine, vaccines and other products of interest in health area, for any disease, requires several in vivo tests using animal models on experiments for clinical analysis of actions in organism, focusing on the relation between these and the responses or reactions to their use, allowing or not their use in human being. The present investigation deals with the determination of elements concentration (Ca, Cl, K, Mg and Na) of clinical relevance in kidney and liver of C57BL/6J mice strain using the Instrumental Neutron Activation Analysis technique. Particularly, the C57BL/6J strain is one of the most widely used mice genetically modified for human disease studies. The biological samples were collected from 2 month old adult mice bred in the Biotherium (animal breeding) of UNIFESP (Federal University of Sao Paulo, Brasil) and at Human Genome Research Center (University of Sao Paulo, Brasil) and Biotechnology Center (IPEN, Sao Paulo, Brasil). The measurements were performed in the nuclear reactor IEA-R1 (3.5-4.5MW, pool type) at IPEN. These data will allow researchers to optimize their studies, both in terms of cost and time, by knowing the basal reference values in blood and organs of this strain. Additionally, this analytical procedure meets the needs of the world tendency that emphasizes the requirements to propose alternative methods for clinical research that contribute to animal welfare. (author)

  9. The application of near-infrared spectra micro-image in the imaging analysis of biology samples

    Directory of Open Access Journals (Sweden)

    Dong Wang

    2014-07-01

    Full Text Available In this research, suitable imaging methods were used for acquiring single compound images of biology samples of chicken pectorales tissue section, tobacco dry leaf, fresh leaf and plant glandular hair, respectively. The adverse effects caused by the high water content and the thermal effect of near infrared (NIR light were effectively solved during the experiment procedures and the data processing. PCA algorithm was applied to the NIR micro-image of chicken pectorales tissue. Comparing the loading vector of PC3 with the NIR spectrum of dry albumen, the information of PC3 was confirmed to be provided mainly by protein, i.e., the 3rd score image represents the distribution trend of protein mainly. PCA algorithm was applied to the NIR micro-image of tobacco dry leaf. The information of PC2 was confirmed to be provided by carbohydrate including starch mainly. Compared to the 2nd score image of tobacco dry leaf, the compared correlation image with the reference spectrum of starch had the same distribution trend as the 2nd score image. The comparative correlation images with the reference spectra of protein, glucose, fructose and the total plant alkaloid were acquired to confirm the distribution trend of these compounds in tobacco dry leaf respectively. Comparative correlation images of fresh leaf with the reference spectra of protein, starch, fructose, glucose and water were acquired to confirm the distribution trend of these compounds in fresh leaf. Chemimap imaging of plant glandular hair was acquired to show the tubular structure clearly.

  10. Exodisc for Rapid, Size-Selective, and Efficient Isolation and Analysis of Nanoscale Extracellular Vesicles from Biological Samples.

    Science.gov (United States)

    Woo, Hyun-Kyung; Sunkara, Vijaya; Park, Juhee; Kim, Tae-Hyeong; Han, Ja-Ryoung; Kim, Chi-Ju; Choi, Hyun-Il; Kim, Yoon-Keun; Cho, Yoon-Kyoung

    2017-02-28

    Extracellular vesicles (EVs) are cell-derived, nanoscale vesicles that carry nucleic acids and proteins from their cells of origin and show great potential as biomarkers for many diseases, including cancer. Efficient isolation and detection methods are prerequisites for exploiting their use in clinical settings and understanding their physiological functions. Here, we presented a rapid, label-free, and highly sensitive method for EV isolation and quantification using a lab-on-a-disc integrated with two nanofilters (Exodisc). Starting from raw biological samples, such as cell-culture supernatant (CCS) or cancer-patient urine, fully automated enrichment of EVs in the size range of 20-600 nm was achieved within 30 min using a tabletop-sized centrifugal microfluidic system. Quantitative tests using nanoparticle-tracking analysis confirmed that the Exodisc enabled >95% recovery of EVs from CCS. Additionally, analysis of mRNA retrieved from EVs revealed that the Exodisc provided >100-fold higher concentration of mRNA as compared with the gold-standard ultracentrifugation method. Furthermore, on-disc enzyme-linked immunosorbent assay using urinary EVs isolated from bladder cancer patients showed high levels of CD9 and CD81 expression, suggesting that this method may be potentially useful in clinical settings to test urinary EV-based biomarkers for cancer diagnostics.

  11. An introduction to the technique of combined ion mobility spectrometry-mass spectrometry for the analysis of complex biological samples

    International Nuclear Information System (INIS)

    McDowall, Mark A.; Bateman, Robert H.; Bajic, Steve; Giles, Kevin; Langridge, Jim; McKenna, Therese; Pringle, Steven D.; Wildgoose, Jason L.

    2008-01-01

    Full Text: Ultra Performance Liquid Chromatography (UPLC) offers several advantages compared with conventional High Performance Liquid Chromatography (HPLC) as an 'inlet system' for mass spectrometry. UPLC provides improved chromatographic resolution, increased sensitivity and reduced analysis time. This is achieved through the use of sub 2μm particles (stationary phase) combined with high-pressure solvent delivery (up to 15,000 psi). When coupled with orthogonal acceleration time-of-flight (oa-TOF) mass spectrometry (MS), UPLC presents a means to achieve high sample throughput with reduced spectral overlap, increased sensitivity, and exact mass measurement capabilities with high mass spectral resolution (Ca 20,000 FWHM). Dispersive ion mobility spectrometry (IMS) implemented within a traveling-wave ion guide provides an orthogonal separation strategy for ions in the gas phase that can resolve isobaric ions formed by either Electrospray of MALDI ionization typically in Ca 20 mille seconds. All three techniques have the potential to be combined on-line (e.g. UPLC-IMS-MS/MS) in real time to maximize peak capacity and resolving power for the analysis of complex biological mixtures including; intact proteins, modified peptides and endogenous/exogenous metabolites

  12. A New Sample Substrate for Imaging and Correlating Organic and Trace Metal Composition in Biological Cells and Tissues

    International Nuclear Information System (INIS)

    Miller, L.; Wang, Q.; Smith, R.; Zhong, H.; Elliott, D.; Warren, J.

    2007-01-01

    Many disease processes involve alterations in the chemical makeup of tissue. Synchrotron-based infrared (IR) and X-ray fluorescence (XRF) microscopes are becoming increasingly popular tools for imaging the organic and trace metal compositions of biological materials, respectively, without the need for extrinsic labels or stains. Fourier transform infrared microspectroscopy (FTIRM) provides chemical information on the organic components of a material at a diffraction-limited spatial resolution of 2-10 μm in the mid-infrared region. The synchrotron X-ray fluorescence (SXRF) microprobe is a complementary technique used to probe trace element content in the same systems with a similar spatial resolution. However to be most beneficial, it is important to combine the results from both imaging techniques on a single sample, which requires precise overlap of the IR and X-ray images. In this work, we have developed a sample substrate containing a gold grid pattern on its surface, which can be imaged with both the IR and X-ray microscopes. The substrate consists of a low trace element glass slide that has a gold grid patterned on its surface, where the major and minor parts of the grid contain 25 and 12 nm gold, respectively. This grid pattern can be imaged with the IR microscope because the reflectivity of gold differs as a function of thickness. The pattern can also be imaged with the SXRF microprobe because the Au fluorescence intensity changes with gold thickness. The tissue sample is placed on top of the patterned substrate. The grid pattern's IR reflectivity image and the gold SXRF image are used as fiducial markers for spatially overlapping the IR and SXRF images from the tissue. Results show that IR and X-ray images can be correlated precisely, with a spatial resolution of less than one pixel (i.e., 2-3 microns). The development of this new tool will be presented along with applications to paraffin-embedded metalloprotein crystals, Alzheimer's disease, and hair

  13. Matrix effects break the LC behavior rule for analytes in LC-MS/MS analysis of biological samples.

    Science.gov (United States)

    Fang, Nianbai; Yu, Shanggong; Ronis, Martin Jj; Badger, Thomas M

    2015-04-01

    High-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) are generally accepted as the preferred techniques for detecting and quantitating analytes of interest in biological matrices on the basis of the rule that one chemical compound yields one LC-peak with reliable retention time (Rt.). However, in the current study, we have found that under the same LC-MS conditions, the Rt. and shape of LC-peaks of bile acids in urine samples from animals fed dissimilar diets differed significantly among each other. To verify this matrix effect, 17 authentic bile acid standards were dissolved in pure methanol or in methanol containing extracts of urine from pigs consuming either breast milk or infant formula and analyzed by LC-MS/MS. The matrix components in urine from piglets fed formula significantly reduced the LC-peak Rt. and areas of bile acids. This is the first characterization of this matrix effect on Rt. in the literature. Moreover, the matrix effect resulted in an unexpected LC behavior: one single compound yielded two LC-peaks, which broke the rule of one LC-peak for one compound. The three bile acid standards which exhibited this unconventional LC behavior were chenodeoxycholic acid, deoxycholic acid, and glycocholic acid. One possible explanation for this effect is that some matrix components may have loosely bonded to analytes, which changed the time analytes were retained on a chromatography column and interfered with the ionization of analytes in the MS ion source to alter the peak area. This study indicates that a comprehensive understanding of matrix effects is needed towards improving the use of HPLC and LC-MS/MS techniques for qualitative and quantitative analyses of analytes in pharmacokinetics, proteomics/metabolomics, drug development, and sports drug testing, especially when LC-MS/MS data are analyzed by automation software where identification of an analyte is based on its exact molecular weight and Rt

  14. Three-dimensional temperature fields of the North Patagonian Sea recorded by Magellanic penguins as biological sampling platforms

    Science.gov (United States)

    Sala, Juan E.; Pisoni, Juan P.; Quintana, Flavio

    2017-04-01

    Temperature is a primary determinant of biogeographic patterns and ecosystem processes. Standard techniques to study the ocean temperature in situ are, however, particularly limited by their time and spatial coverage, problems which might be partially mitigated by using marine top predators as biological platforms for oceanographic sampling. We used small archival tags deployed on 33 Magellanic penguins (Spheniscus magellanicus), and obtained 21,070 geo-localized profiles of water temperature, during late spring of 2008, 2011, 2012 and 2013; in a region of the North Patagonian Sea with limited oceanographic records in situ. We compared our in situ data of sea surface temperature (SST) with those available from satellite remote sensing; to describe the three-dimensional temperature fields around the area of influence of two important tidal frontal systems; and to study the inter-annual variation in the three-dimensional temperature fields. There was a strong positive relationship between satellite- and animal-derived SST data although there was an overestimation by remote-sensing by a maximum difference of +2 °C. Little inter-annual variability in the 3-dimensional temperature fields was found, with the exception of 2012 (and to a lesser extent in 2013) where the SST was significantly higher. In 2013, we found weak stratification in a region which was unexpected. In addition, during the same year, a warm small-scale vortex is indicated by the animal-derived temperature data. This allowed us to describe and better understand the dynamics of the water masses, which, so far, have been mainly studied by remote sensors and numerical models. Our results highlight again the potential of using marine top predators as biological platforms to collect oceanographic data, which will enhance and accelerate studies on the Southwest Atlantic Ocean. In a changing world, threatened by climate change, it is urgent to fill information gaps on the coupled ocean-atmosphere system

  15. FACE Analysis as a Fast and Reliable Methodology to Monitor the Sulfation and Total Amount of Chondroitin Sulfate in Biological Samples of Clinical Importance

    Directory of Open Access Journals (Sweden)

    Evgenia Karousou

    2014-06-01

    Full Text Available Glycosaminoglycans (GAGs due to their hydrophilic character and high anionic charge densities play important roles in various (pathophysiological processes. The identification and quantification of GAGs in biological samples and tissues could be useful prognostic and diagnostic tools in pathological conditions. Despite the noteworthy progress in the development of sensitive and accurate methodologies for the determination of GAGs, there is a significant lack in methodologies regarding sample preparation and reliable fast analysis methods enabling the simultaneous analysis of several biological samples. In this report, developed protocols for the isolation of GAGs in biological samples were applied to analyze various sulfated chondroitin sulfate- and hyaluronan-derived disaccharides using fluorophore-assisted carbohydrate electrophoresis (FACE. Applications to biologic samples of clinical importance include blood serum, lens capsule tissue and urine. The sample preparation protocol followed by FACE analysis allows quantification with an optimal linearity over the concentration range 1.0–220.0 µg/mL, affording a limit of quantitation of 50 ng of disaccharides. Validation of FACE results was performed by capillary electrophoresis and high performance liquid chromatography techniques.

  16. Inalienably Yours? The new case for an inalienable property right in human biological material: Empowerment of sample donors or a recipe for a tragic Anti-Commons?

    Directory of Open Access Journals (Sweden)

    Jasper A. Bovenberg

    2004-12-01

    Full Text Available Modern biomedical research into the genetic component of common diseases calls for broad access to existing and novel collections of samples of human biological material, aka Biobanks. Groups of donors of these samples, however, increasingly claim a property right in their samples. They perceive the recognition of a personal property right in their biological material as the best means to serve two goals: to secure ongoing control over their samples after donation and to underpin their claim for a share in the proceeds that the research on their samples may yield. Given the objective of ensuring ongoing control, this property right is claimed to be inalienable. Recognition of a personal property right in one’s biological material is problematic, especially where the requirement of inalienability seems at odds with the claim for a share of the profits. Yet, property rights in human biological material may be justified in a certain context, e.g. to enable subsets of patients to negotiate the terms and conditions of the research into their specific disorders. Biobanks, however, contain so many samples, which can be used for so many research purposes, that the unrestricted exercise of personal property rights by the sample donors will lead to a proliferation of rights. This proliferation is likely to deter or slow down both the creation of de novo Biobanks and the use of existing sample collections. Thus, recognising inalienable property rights in human biological material may lead to suboptimal use of these resources and create a classic ‘anticommons property’ scenario. It would also undermine the current trend to simplify existing informed consent requirements which aims to facilitate broad and previously unanticipated research on de novo and existing Biobanks. In addition, the tradition of altruistic participation in research and the notion that large-scale collections of human biological material are global public goods are arguments against

  17. Field-based detection of biological samples for forensic analysis: Established techniques, novel tools, and future innovations.

    Science.gov (United States)

    Morrison, Jack; Watts, Giles; Hobbs, Glyn; Dawnay, Nick

    2018-02-21

    Field based forensic tests commonly provide information on the presence and identity of biological stains and can also support the identification of species. Such information can support downstream processing of forensic samples and generate rapid intelligence. These approaches have traditionally used chemical and immunological techniques to elicit the result but some are known to suffer from a lack of specificity and sensitivity. The last 10 years has seen the development of field-based genetic profiling systems, with specific focus on moving the mainstay of forensic genetic analysis, namely STR profiling, out of the laboratory and into the hands of the non-laboratory user. In doing so it is now possible for enforcement officers to generate a crime scene DNA profile which can then be matched to a reference or database profile. The introduction of these novel genetic platforms also allows for further development of new molecular assays aimed at answering the more traditional questions relating to body fluid identity and species detection. The current drive for field-based molecular tools is in response to the needs of the criminal justice system and enforcement agencies, and promises a step-change in how forensic evidence is processed. However, the adoption of such systems by the law enforcement community does not represent a new strategy in the way forensic science has integrated previous novel approaches. Nor do they automatically represent a threat to the quality control and assurance practices that are central to the field. This review examines the historical need and subsequent research and developmental breakthroughs in field-based forensic analysis over the past two decades with particular focus on genetic methods Emerging technologies from a range of scientific fields that have potential applications in forensic analysis at the crime scene are identified and associated issues that arise from the shift from laboratory into operational field use are discussed

  18. Evaluation of calcium, magnesium, potassium and sodium in biological samples of male human immunodeficiency virus patients with tuberculosis and diarrhea compared to healthy control subjects in Pakistan.

    Science.gov (United States)

    Afridi, Hassan Imran; Kazi, Tasneem Gul; Talpur, Farah Naz; Kazi, Naveed; Naeemullah, Faheem Shah; Arain, Sadaf Sadia; Brahman, Kapil Dev

    2013-01-01

    Electrolyte deficiency has been associated with an increased risk of human immunodeficiency virus type 1 (HIV-1) disease progression and mortality. This study examined the association between low electrolyte concentrations in blood and scalp hair and the presence of opportunistic infections in patients with acquired immune deficiency syndrome (AIDS). Sixty-two male HIV positive patients (HIV-1) from various cities in Pakistan were recruited to the study. These Patients were divided into two groups according to secondary infections (tuberculosis and high fever with diarrhea), and biological samples (scalp hair, serum, blood and urine) were collected from them. As a comparative control group, 120 healthy subjects (males) of the same age group (31 - 45 years), socio-economic status, localities and dietary habits were also included in the study. The elements in the biological samples were analyzed by flame atomic absorption spectrophotometry after microwave-assisted acid digestion. Validity and accuracy of the methodology were checked using certified reference materials (CRMs) and against values obtained by a conventional wet acid digestion method on the same CRMs. The results indicated significantly lower levels of calcium, potassium, magnesium and natrium in all analyzed biological samples (blood, serum and scalp hair) of male patients with Acquired Immune Deficiency Syndrome (AIDS) in comparison to healthy controls (p urine samples of the AIDS patients than in those of the control group. These data offer guidance to clinicians and other professionals investigating the deficiency of electrolytes in biological samples (scalp hair, serum and blood) of AIDS patients in relation to healthy subjects.

  19. Explanation, understanding, and unrealistic models

    NARCIS (Netherlands)

    Hindriks, Frank

    How can false models be explanatory? And how can they help us to understand the way the world works? Sometimes scientists have little hope of building models that approximate the world they observe. Even in such cases, I argue, the models they build can have explanatory import. The basic idea is

  20. Polymer monolithic capillary microextraction combined on-line with inductively coupled plasma MS for the determination of trace rare earth elements in biological samples.

    Science.gov (United States)

    Zhang, Lin; Chen, Beibei; He, Man; Hu, Bin

    2013-07-01

    A rapid and sensitive method based on polymer monolithic capillary microextraction combined on-line with microconcentric nebulization inductively coupled plasma MS has been developed for the determination of trace/ultratrace rare earth elements in biological samples. For this purpose, the iminodiacetic acid modified poly(glycidyl methacrylate-trimethylolpropane trimethacrylate) monolithic capillary was prepared and characterized by SEM and FTIR spectroscopy. Factors affecting the extraction efficiency, such as sample pH, sample flow rate, sample/eluent volume, and coexisting ions were investigated in detail. Under the optimal conditions, the LODs for rare earth elements were in the range of 0.08 (Er) to 0.97 ng/L (Nd) with a sampling frequency of 8.5 h(-1), and the RSDs were between 1.5% (Sm) and 7.4% (Nd) (c = 20 ng/L, n = 7). The proposed method was successfully applied to the analysis of trace/ultratrace rare earth elements in human urine and serum samples, and the recoveries for the spiked samples were in the range of 82-105%. The developed method was simple, rapid, sensitive, and favorable for the analysis of trace/ultratrace rare earth elements in biological samples with limited sample volume. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. The use of double laser pulses for the atomic-emission spectral estimation of uranium content in biological samples

    International Nuclear Information System (INIS)

    Patapovich, M.P.; Umreiko, D.S.; Zajogin, A.P.; Buloichik, J.I.

    2012-01-01

    This paper is aimed at the development of the techniques for estimation of the uranium content in biological objects (hair) using the atomic-emission laser analysis with a sufficient accuracy and high processing rate. (authors)

  2. Solid-phase extraction followed by dispersive liquid-liquid microextraction for the sensitive determination of ecstasy compounds and amphetamines in biological samples

    Directory of Open Access Journals (Sweden)

    H. A. Mashayekhi

    2014-09-01

    Full Text Available A novel approach for the determination of ecstasy and amphetamines (3,4-methylenedioxymethylamphetamine (MDMA, Ecstasy, 3,4-methylenedioxyamphetamine (MDA, 3,4-methylenedioxyethylamphetamine (MDEA and 3,4-methylenedioxypropylamphetamine (MDPA in biological samples is presented. The analytes were extracted from the matrix and transferred to a small volume of a high density, water insoluble solvent using solid-phase extraction (SPE followed by dispersive liquid-liquid microextraction (DLLME. This combination not only resulted in a high enrichment factor, but also it could be used in complex matrices (biological samples. Some important extraction parameters, such as sample solution flow rate, sample pH, type and volume of extraction and disperser solvents as well as the salt addition, were studied and optimized. Under the optimized conditions, the calibration graphs were linear in the range of 0.5-500 µg L-1 and 1.0-500 µg L-1 with detection limits in the range of 0.1-0.3 µg L-1 and 0.2-0.7 µg L-1 in urine and plasma samples, respectively. The results showed that SPE-DLLME is a suitable method for the determination of ecstasy components and amphetamines in biological and water samples. DOI: http://dx.doi.org/10.4314/bcse.v28i3.3

  3. The use of high energy laser-plasma sources in soft X-ray contact microscopy of living biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Batani, D.; Botto, C.; Moret, M.; Milani, M.; Lucchini, G. [Universita degli Studi di Milano-Bicocca and INFM, Milano (Italy); Eidmann, K. [Max-Planck-Institut fuer Quantenoptik, Garching (Germany); Cotelli, F.; Lora Lamia Donin, C.; Poletti, G. [Universita di Milano (Italy); Ford, T.; Stead, A. [London Univ., Royal Holloway (United Kingdom)

    2002-11-01

    In this paper the results of an experiment on soft X-ray contact microscopy using a laser-plasma source are presented. A resolution of 50 nm has been achieved imaging pig sperm cells, while other specimens, such as algae and yeast cells, showed internal details, proving the technique to be a powerful tool for biological investigations. Original biological information has been obtained and the conditions for optimal image formation have been studied. (authors)

  4. Experiences performed at the C:R: Saluggia of ENEA in low-level determination of plutonium in biological and environmental samples

    International Nuclear Information System (INIS)

    Spezzano, Pasquale

    1997-10-01

    This report describes some experiences performed at the Research Center Saluggia of ENEA concerning low-level determination of plutonium in biological and environmental samples, with discussions of practical analytical problems. The main characteristics and properties of plutonium with emphasis to aqueous solutions chemistry and environmental behaviour are also reported

  5. Biological validation of a sample preparation method for ER-CALUX bioanalysis of estrogenic activity in sediments using mixtures of xeno-estrogens

    NARCIS (Netherlands)

    Houtman, C.J.; Houten, Y.K.; Leonards, P.E.G.; Brouwer, A.; Lamoree, M.H.; Legler, J.

    2006-01-01

    The combined estrogenic effects of mixtures of environmental pollutants in the in vitro ER-CALUX (chemical activated luciferase gene expression) bioassay were examined to biologically validate a sample preparation method for the analysis of estrogenic compounds in sediment. The method used

  6. On-line coupling of solid-phase extraction with mass spectrometry for the analysis of biological samples I. Determination of clenbuterol in urine

    NARCIS (Netherlands)

    Bruins, C.H P; Jeronimus-Stratingh, C.M; Ensing, K; van Dongen, W.D; de Jong, G.J.

    1999-01-01

    The potential of the direct coupling of solid-phase extraction (SPE) with mass spectrometry (MS) for the analysis of biological samples is demonstrated. For SPE a cartridge exchanger is used and the eluate is directly introduced into the mass spectrometer. This system has been investigated for the

  7. Gene-ontology enrichment analysis in two independent family-based samples highlights biologically plausible processes for autism spectrum disorders.

    LENUS (Irish Health Repository)

    Anney, Richard J L

    2012-02-01

    Recent genome-wide association studies (GWAS) have implicated a range of genes from discrete biological pathways in the aetiology of autism. However, despite the strong influence of genetic factors, association studies have yet to identify statistically robust, replicated major effect genes or SNPs. We apply the principle of the SNP ratio test methodology described by O\\'Dushlaine et al to over 2100 families from the Autism Genome Project (AGP). Using a two-stage design we examine association enrichment in 5955 unique gene-ontology classifications across four groupings based on two phenotypic and two ancestral classifications. Based on estimates from simulation we identify excess of association enrichment across all analyses. We observe enrichment in association for sets of genes involved in diverse biological processes, including pyruvate metabolism, transcription factor activation, cell-signalling and cell-cycle regulation. Both genes and processes that show enrichment have previously been examined in autistic disorders and offer biologically plausibility to these findings.

  8. Rapid, simple, and highly sensitive analysis of drugs in biological samples using thin-layer chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry.

    Science.gov (United States)

    Kuwayama, Kenji; Tsujikawa, Kenji; Miyaguchi, Hajime; Kanamori, Tatsuyuki; Iwata, Yuko T; Inoue, Hiroyuki

    2012-01-01

    Rapid and precise identification of toxic substances is necessary for urgent diagnosis and treatment of poisoning cases and for establishing the cause of death in postmortem examinations. However, identification of compounds in biological samples using gas chromatography and liquid chromatography coupled with mass spectrometry entails time-consuming and labor-intensive sample preparations. In this study, we examined a simple preparation and highly sensitive analysis of drugs in biological samples such as urine, plasma, and organs using thin-layer chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry (TLC/MALDI/MS). When the urine containing 3,4-methylenedioxymethamphetamine (MDMA) without sample dilution was spotted on a thin-layer chromatography (TLC) plate and was analyzed by TLC/MALDI/MS, the detection limit of the MDMA spot was 0.05 ng/spot. The value was the same as that in aqueous solution spotted on a stainless steel plate. All the 11 psychotropic compounds tested (MDMA, 4-hydroxy-3-methoxymethamphetamine, 3,4-methylenedioxyamphetamine, methamphetamine, p-hydroxymethamphetamine, amphetamine, ketamine, caffeine, chlorpromazine, triazolam, and morphine) on a TLC plate were detected at levels of 0.05-5 ng, and the type (layer thickness and fluorescence) of TLC plate did not affect detection sensitivity. In addition, when rat liver homogenate obtained after MDMA administration (10 mg/kg) was spotted on a TLC plate, MDMA and its main metabolites were identified using TLC/MALDI/MS, and the spots on a TLC plate were visualized by MALDI/imaging MS. The total analytical time from spotting of intact biological samples to the output of analytical results was within 30 min. TLC/MALDI/MS enabled rapid, simple, and highly sensitive analysis of drugs from intact biological samples and crude extracts. Accordingly, this method could be applied to rapid drug screening and precise identification of toxic substances in poisoning cases and

  9. Development of a Univariate Membrane-Based Mid-Infrared Method for Protein Quantitation and Total Lipid Content Analysis of Biological Samples

    Directory of Open Access Journals (Sweden)

    Ivona Strug

    2014-01-01

    Full Text Available Biological samples present a range of complexities from homogeneous purified protein to multicomponent mixtures. Accurate qualification of such samples is paramount to downstream applications. We describe the development of an MIR spectroscopy-based analytical method offering simultaneous protein quantitation (0.25–5 mg/mL and analysis of total lipid or detergent species, as well as the identification of other biomolecules present in biological samples. The method utilizes a hydrophilic PTFE membrane engineered for presentation of aqueous samples in a dried format compatible with fast infrared analysis. Unlike classical quantification techniques, the reported method is amino acid sequence independent and thus applicable to complex samples of unknown composition. By comparison to existing platforms, this MIR-based method enables direct quantification using minimal sample volume (2 µL; it is well-suited where repeat access and limited sample size are critical parameters. Further, accurate results can be derived without specialized training or knowledge of IR spectroscopy. Overall, the simplified application and analysis system provides a more cost-effective alternative to high-throughput IR systems for research laboratories with minimal throughput demands. In summary, the MIR-based system provides a viable alternative to current protein quantitation methods; it also uniquely offers simultaneous qualification of other components, notably lipids and detergents.

  10. Prediction uncertainty assessment of a systems biology model requires a sample of the full probability distribution of its parameters

    NARCIS (Netherlands)

    Mourik, van S.; Braak, ter C.J.F.; Stigter, J.D.; Molenaar, J.

    2014-01-01

    Multi-parameter models in systems biology are typically ‘sloppy’: some parameters or combinations of parameters may be hard to estimate from data, whereas others are not. One might expect that parameter uncertainty automatically leads to uncertain predictions, but this is not the case. We illustrate

  11. Matrix effects break the LC behavior rule for analytes in LC-MS/MS analysis of biological samples

    Science.gov (United States)

    High-performance liquid chromatography (HPLC) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) are generally accepted as the preferred techniques for detecting and quantitating analytes of interest in biological matrices on the basis of the rule that one chemical compound yields one LC-...

  12. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection.

    Science.gov (United States)

    Jaszczak, Ewa; Ruman, Marek; Narkowicz, Sylwia; Namieśnik, Jacek; Polkowska, Żaneta

    2017-01-01

    A simple and accurate ion chromatography (IC) method with pulsed amperometric detection (PAD) was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1-100  μ g/L for urine, 5-100  μ g/L for saliva, and 3-100  μ g/L for sweat samples with determination coefficients ( R ) > 0.992. Low detection limits (LODs) in the range of 1.8  μ g/L, 5.1  μ g/L, and 5.8  μ g/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n = 3) were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

  13. Development of an Analytical Protocol for Determination of Cyanide in Human Biological Samples Based on Application of Ion Chromatography with Pulsed Amperometric Detection

    Directory of Open Access Journals (Sweden)

    Ewa Jaszczak

    2017-01-01

    Full Text Available A simple and accurate ion chromatography (IC method with pulsed amperometric detection (PAD was proposed for the determination of cyanide ion in urine, sweat, and saliva samples. The sample pretreatment relies on alkaline digestion and application of Dionex OnGuard II H cartridge. Under the optimized conditions, the method showed good linearity in the range of 1–100 μg/L for urine, 5–100 μg/L for saliva, and 3–100 μg/L for sweat samples with determination coefficients (R>0.992. Low detection limits (LODs in the range of 1.8 μg/L, 5.1 μg/L, and 5.8 μg/L for urine, saliva, and sweat samples, respectively, and good repeatability (CV < 3%, n=3 were obtained. The proposed method has been successfully applied to the analysis of human biological samples.

  14. Recommendations for sampling for prevention of hazards in civil defense. On analytics of chemical, biological and radioactive contaminations. 2. ed.; Empfehlungen fuer die Probenahme zur Gefahrenabwehr im Bevoelkerungsschutz. Zur Analytik von chemischen, biologischen und radioaktiven Kontaminationen

    Energy Technology Data Exchange (ETDEWEB)

    Bachmann, Udo; Derakshani, Nahid; Drobig, Matthias; Koenig, Mario; Mentfewitz, Joachim; Prast, Hartmut; Uelpenich, Gerhard; Vidmayer, Marc; Wilbert, Stefan; Wolf, Manfred

    2016-07-01

    The recommendations for sampling for prevention of hazards in civil defense (analytics of chemical, biological and radioactive contaminations) cover the following topics: Requirements for sampling, description of the materials (chemical, biological and radioactive contaminated materials), decontamination, sample transport and protocol documents.

  15. QChIPat: a quantitative method to identify distinct binding patterns for two biological ChIP-seq samples in different experimental conditions.

    Science.gov (United States)

    Liu, Bin; Yi, Jimmy; Sv, Aishwarya; Lan, Xun; Ma, Yilin; Huang, Tim H M; Leone, Gustavo; Jin, Victor X

    2013-01-01

    Many computational programs have been developed to identify enriched regions for a single biological ChIP-seq sample. Given that many biological questions are often asked to compare the difference between two different conditions, it is important to develop new programs that address the comparison of two biological ChIP-seq samples. Despite several programs designed to address this question, these programs suffer from some drawbacks, such as inability to distinguish whether the identified differential enriched regions are indeed significantly enriched, lack of distinguishing binding patterns, and neglect of the normalization between samples. In this study, we developed a novel quantitative method for comparing two biological ChIP-seq samples, called QChIPat. Our method employs a new global normalization method: nonparametric empirical Bayes (NEB) correction normalization, utilizes pre-defined enriched regions identified from single-sample peak calling programs, uses statistical methods to define differential enriched regions, then defines binding (histone modification) pattern information for those differential enriched regions. Our program was tested on a benchmark data: histone modifications data used by ChIPDiffs. It was then applied on two study cases: one to identify differential histone modification sites for ChIP-seq of H3K27me3 and H3K9me2 data in AKT1-transfected MCF10A cells; the other to identify differential binding sites for ChIP-seq of TCF7L2 data in MCF7 and PANC1 cells. Several advantages of our program include: 1) it considers a control (or input) experiment; 2) it incorporates a novel global normalization strategy: nonparametric empirical Bayes correction normalization; 3) it provides the binding pattern information among different enriched regions. QChIPat is implemented in R, Perl and C++, and has been tested under Linux. The R package is available at http://motif.bmi.ohio-state.edu/QChIPat.

  16. High sensitivity and selectivity in quantitative analysis of drugs in biological samples using 4-column multidimensional micro-UHPLC-MS enabling enhanced sample loading capacity.

    Science.gov (United States)

    de Vries, Ronald; Vereyken, Liesbeth; François, Isabelle; Dillen, Lieve; Vreeken, Rob J; Cuyckens, Filip

    2017-10-09

    Sensitivity is often a critical parameter in quantitative bioanalyses in drug development. For liquid-chromatography-based methods, sensitivity can be improved by reducing the column diameter, but practical sensitivity gains are limited by the reduced sample loading capacity on small internal diameter (I.D.) columns. We developed a set-up that has overcome these limitations in sample loading capacity. The set-up uses 4 columns with gradually decreasing column diameters along the flow-path (2.1 → 1 → 0.5 → 0.15 mm). Samples are pre-concentrated on-line on a 2.1 mm I.D. trapping column and back flushed to a 1 mm I.D. UHPLC analytical column and separated. The peak(s) of interest are transferred using heartcutting to a second trapping column (0.5 mm I.D.), which is back-flushed to a 0.15 mm I.D. micro-UHPLC analytical column for orthogonal separation. The proof of concept of the set-up was demonstrated by the simultaneous analysis of midazolam and 1'-hydroxy midazolam in plasma by injection of 80 μL of protein precipitated plasma. The 4-column funnel set-up proved to be robust and resulted in a 10-50 times better sensitivity compared to a trap-elute approach and 250-500 fold better compared to direct micro-UHPLC analysis. A lower limit of quantification of 100 fg/mL in plasma was obtained for both probe compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

  17. Comparison Of INAA Methods (Long Conventional, Cyclic And Pseudo-Cyclic) For The Determination Of Se In Biological Samples

    International Nuclear Information System (INIS)

    Sarheel, A.

    2004-01-01

    Selenium content in serum blood, sample were received from international comparison programme (SABC) has been determined by Cyclic irradiation, pseudo-cyclic irradiation and long irradiation conventional Instrumental neutron activation analysis through the 162 keV gamma ray of the 77m Se nuclide for both cyclic and pseudo-cyclic and 264 keV gamma ray of 75 Se nuclide for conventional (long irradiation). The CINAA involve irradiation of samples for 20 s, decay for 15 s and counting for 20 s, samples recycling four times to improve the precision. The PCINAA involve irradiation of samples for 20 s, decay for 20 s and counting for 30s, samples recycling four times day by day. The Conventional (long irradiation) involve irradiation of samples for 20 hr (1 week), decay for 4 weeks and counting for 20 hr. The accuracy has been evaluated by analyzing the certified reference materials. (Author)

  18. Cryogenic coherent X-ray diffraction imaging of biological samples at SACLA: a correlative approach with cryo-electron and light microscopy.

    Science.gov (United States)

    Takayama, Yuki; Yonekura, Koji

    2016-03-01

    Coherent X-ray diffraction imaging at cryogenic temperature (cryo-CXDI) allows the analysis of internal structures of unstained, non-crystalline, whole biological samples in micrometre to sub-micrometre dimensions. Targets include cells and cell organelles. This approach involves preparing frozen-hydrated samples under controlled humidity, transferring the samples to a cryo-stage inside a vacuum chamber of a diffractometer, and then exposing the samples to coherent X-rays. Since 2012, cryo-coherent diffraction imaging (CDI) experiments have been carried out with the X-ray free-electron laser (XFEL) at the SPring-8 Ångstrom Compact free-electron LAser (SACLA) facility in Japan. Complementary use of cryo-electron microscopy and/or light microscopy is highly beneficial for both pre-checking samples and studying the integrity or nature of the sample. This article reports the authors' experience in cryo-XFEL-CDI of biological cells and organelles at SACLA, and describes an attempt towards reliable and higher-resolution reconstructions, including signal enhancement with strong scatterers and Patterson-search phasing.

  19. Simultaneous multi-species determination of trimethyllead, monomethylmercury and three butyltin compounds by species-specific isotope dilution GC-ICP-MS in biological samples.

    Science.gov (United States)

    Poperechna, Nataliya; Heumann, Klaus G

    2005-09-01

    An accurate and sensitive multi-species species-specific isotope dilution GC-ICP-MS method was developed for the simultaneous determination of trimethyllead (Me3Pb+), monomethylmercury (MeHg+) and the three butyltin species Bu3Sn+, Bu2Sn2+, and BuSn3+ in biological samples. The method was validated by three biological reference materials (CRM 477, mussel tissue certified for butyltins; CRM 463, tuna fish certified for MeHg+; DORM 2, dogfish muscle certified for MeHg+). Under certain conditions, and with minor modifications of the sample pretreatment procedure, this method could also be transferred to environmental samples such as sediments, as demonstrated by analyzing sediment reference material BCR 646 (freshwater sediment, certified for butyltins). The detection limits of the multi-species GC-ICP-IDMS method for biological samples were 1.4 ng g(-1) for MeHg+, 0.06 ng g(-1) for Me3Pb+, 0.3 ng g(-1) for BuSn3+ and Bu3Sn+, and 1.2 ng g(-1) for Bu2Sn2+. Because of the high relevance of these heavy metal alkyl species to the quality assurance of seafood, the method was also applied to corresponding samples purchased from a supermarket. The methylated lead fraction in these samples, correlated to total lead, varied over a broad range (from 0.01% to 7.6%). On the other hand, the MeHg+ fraction was much higher, normally in the range of 80-100%. Considering that we may expect tighter legislative limitations on MeHg+ levels in seafood in the future, we found the highest methylmercury contents (up to 10.6 microg g(-1)) in two shark samples, an animal which is at the end of the marine food chain, whereas MeHg+ contents of less than 0.2 microg g(-1) were found in most other seafood samples; these results correlate with the idea that MeHg+ is usually of biological origin in the marine environment. The concentration of butyltins and the fraction of the total tin content that is from butyltins strongly depend on possible contamination, due to the exclusively anthropogenic

  20. Automated extraction of DNA from reference samples from various types of biological materials on the Qiagen BioRobot EZ1 Workstation

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Jørgensen, Mads; Hansen, Anders Johannes

    2009-01-01

    We have validated and implemented a protocol for DNA extraction from various types of biological materials using a Qiagen BioRobot EZ1 Workstation. The sample materials included whole blood, blood from deceased, buccal cells on Omni swabs and FTA Cards, blood on FTA Cards and cotton swabs......, and muscle biopsies. The DNA extraction was validated according to EN/ISO 17025 for the STR kits AmpFlSTR« Identifiler« and AmpFlSTR« Yfiler« (Applied Biosystems). Of 298 samples extracted, 11 (4%) did not yield acceptable results. In conclusion, we have demonstrated that extraction of DNA from various types...... of biological material can be performed quickly and without the use of hazardous chemicals, and that the DNA may be successfully STR typed according to the requirements of forensic genetic investigations accredited according to EN/ISO 17025...

  1. Implementation challenges to using respondent-driven sampling methodology for HIV biological and behavioral surveillance: field experiences in international settings.

    Science.gov (United States)

    Johnston, Lisa Grazina; Malekinejad, Mohsen; Kendall, Carl; Iuppa, Irene M; Rutherford, George W

    2008-07-01

    Using respondent-driven sampling (RDS), we gathered data from 128 HIV surveillance studies conducted outside the United States through October 1, 2007. We examined predictors of poor study outcomes, reviewed operational, design and analytical challenges associated with conducting RDS in international settings and offer recommendations to improve HIV surveillance. We explored factors for poor study outcomes using differences in mean sample size ratios (recruited/calculated sample size) as the outcome variable. Ninety-two percent of studies reported both calculated and recruited sample sizes. Studies of injecting drug users had a higher sample size ratio compared with other risk groups. Study challenges included appropriately defining eligibility criteria, structuring social network size questions, selecting design effects and conducting statistical analysis. As RDS is increasingly used for HIV surveillance, it is important to learn from past practical, theoretical and analytical challenges to maximize the utility of this method.

  2. Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

    International Nuclear Information System (INIS)

    Lux, F.; Bereznai, T.; Haeberlin, T.H.

    1986-01-01

    In our determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing we have tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics have been investigated: the abrasions from scalpels made of stainless steel, titanium or quartz; the type of surgery; the homogenisation of the samples before irradiation by use of a ball milll; the surface contaminations of the quartz ampoules that pass into the digestion solution of the irradiated samples. The appropriate measures taken in order to reduce the blank values are described. The results of analyses performed under these conditions indicate the effectiveness of the given measures, especially shown by the low values obtained for the chromium contents of the analysed muscle samples. (author)

  3. Biological Agent Sample Preparation for the Detection and Identification of Multiple Agents by Nucleic Acid-Based Analysis

    National Research Council Canada - National Science Library

    Fields, Robert

    2002-01-01

    .... The AutoLyser instrument which we have developed, provides fully automated purification of viral, bacterial and human genomic DNA and RNA from clinical samples, cell culture and swabs in as little...

  4. Analysis of thyroid hormones in biological samples using stable isotope dilution liquid chromatography-tandem mass spectrometry

    Science.gov (United States)

    This poster presentation will describe analytical chemistry methods for measuring thyroid hormones and related precursors and metabolites in very small tissue or plasma samples. These methods are amenable to measure thyroid hormones in amphibian tadpoles or small mammals used as ...

  5. A full evaporation headspace technique with capillary GC and ITD: a means for quantitating volatile organic compounds in biological samples.

    Science.gov (United States)

    Schuberth, J

    1996-07-01

    The full evaporation technique (FET), which is a variant of headspace analysis used to overcome matrix effects, was combined with capillary gas chromatography (GC) and ion-trap detection (ITD). The aim was to enable quantitative tests of volatile organic compounds (VOCs) in blood and postmortem tissue samples. FET was applied to sample sized less than 35 mg whose VOCs were released from the matrix at an equilibration temperature of 130 degrees C. A capillary column with a nonpolar stationary phase was used for GC, and ITD was performed with the mass spectrometer run in full-scan mode. The potential of FET-GC-ITD was studied for the analysis of blood samples spiked with low concentrations of ethanol, acetone, 2-propanol, and 2-butanone and on brain tissue that contained methyl tert-butyl ether (MTBE), Benzene, toluene, ethylbenzene, o-, m-, and p-xylene, and propylbenzene. Samples were obtained from the bodies of victims who had inhaled smoke during an arson or accidental fire. There was a linear relationship between peak area and sample size, which indicates that the conditions of full evaporation were met and that the matrix effect was negated. The total analyte amount in the test sample at the limit of quantitation was in the range of 0.4-1 nmol for polar VOCs in blood and 0.03-0.1 nmol for nonpolar VOCs in brain tissue. Data on precision and accuracy of the method are reported.

  6. Analysis of sediment, water, and biological samples from the Bay Farm Borrow Area, San Francisco Bay, California

    Energy Technology Data Exchange (ETDEWEB)

    Thom, R.M.; Lefkovitz, L.F. (Battelle/Marine Sciences Lab., Sequim, WA (United States))

    1991-08-01

    The Bay Farm Borrow Area (BFBA) of San Francisco Bay, California, is under consideration as a dredged-material disposal site by the US Army Corps of Engineers (USACE). As part of the analysis of the site, information is required on the quality of benthic biota, sediment, and water in the BFBA. The objective of this report was to provide data on infauna communities, sediment, and water chemistry from samples collected from the BFBA. The samples were collected, and the data will be analyzed by Science Applications International (SAIC). A total of four samples for sediment chemistry, four samples for water chemistry, and 7 samples for infauna communities were analyzed by the Battelle/Marine Sciences Laboratory (MSL). Water analyses included tests for dissolved organic carbon, total suspended solids, four metals, butyltins, polychlorinated biphenyls (PCBs), chlorinated pesticides, polynuclear aromatic hydrocarbons (PAHs), four phenols, and total phenol. Sediment samples were analyzed for percent solids, total organic carbon, total oil and grease, total petroleum hydrocarbons, grain size, 10 metals, butyltins, PCBs, chlorinated pesticides, PAHs, four phenols, and total phenol. The data along with controls and spike recovery analyses, are presented in tables, and the results are discussed in the text. The quality assurance/quality control criteria were met for the analyses as were the detection limits specified by the sponsor.

  7. Quantitative evaluation of freeze-substitution effects on preservation of nuclear antigens during preparation of biological samples for immunoelectron microscopy

    Czech Academy of Sciences Publication Activity Database

    Sobol, Margaryta; Philimonenko, Vlada; Philimonenko, Anatoly; Hozák, Pavel

    2012-01-01

    Roč. 138, č. 1 (2012), s. 167-177 ISSN 0948-6143 R&D Projects: GA AV ČR KAN200520704; GA MŠk 2B06063; GA MŠk LC545; GA ČR GAP305/11/2232 Institutional research plan: CEZ:AV0Z50520514 Keywords : immuno-gold labeling * automated freeze-substitution * LR White * immunohistochemistry * high-pressure freezing Subject RIV: EB - Genetics ; Molecular Biology Impact factor: 2.613, year: 2012

  8. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Zhuomin [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Wang Qingtang [Key Laboratory of Analysis and Detection for Food Safety of Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou, Fujian 350002 (China); Li Gongke, E-mail: cesgkl@mail.sysu.edu.cn [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China)

    2012-05-21

    Highlights: Black-Right-Pointing-Pointer Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. Black-Right-Pointing-Pointer NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. Black-Right-Pointing-Pointer NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7-4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography-mass spectrometry (GC-MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient

  9. Fabrication of novel nanoporous array anodic alumina solid-phase microextraction fiber coating and its potential application for headspace sampling of biological volatile organic compounds

    International Nuclear Information System (INIS)

    Zhang Zhuomin; Wang Qingtang; Li Gongke

    2012-01-01

    Highlights: ► Nanoporous array anodic alumina (NAAA) SPME coating was originally prepared. ► NAAA SPME coating achieved excellent enrichment capability and selectivity for VOCs. ► NAAA SPME coating can be applied for the headspace sampling of biological VOCs. - Abstract: In the study, nanoporous array anodic alumina (NAAA) prepared by a simple, rapid and stable two-step anodic oxidization method was introduced as a novel solid-phase microextraction (SPME) fiber coating. The regular nanoporous array structure and chemical composition of NAAA SPME fiber coating was characterized and validated by scanning electron microscopy and energy dispersive spectroscopy, respectively. Compared with the commercial polydimethylsiloxane (PDMS) SPME fiber coating, NAAA SPME fiber coating achieved the higher enrichment capability (1.7–4.7 folds) for the mixed standards of volatile organic compounds (VOCs). The selectivity for volatile alcohols by NAAA SPME fiber coating demonstrated an increasing trend with the increasing polarity of alcohols caused by the gradually shortening carbon chains from 1-undecanol to 1-heptanol or the isomerization of carbon chains of some typical volatile alcohols including 2-ethyl hexanol, 1-octanol, 2-phenylethanol, 1-phenylethanol, 5-undecanol, 2-undecanol and 1-undecanol. Finally, NAAA SPME fiber coating was originally applied for the analysis of biological VOCs of Bailan flower, stinkbug and orange peel samples coupled with gas chromatography–mass spectrometry (GC–MS) detection. Thirty, twenty-seven and forty-four VOCs of Bailan flower, stinkbug and orange peel samples were sampled and identified, respectively. Moreover, the contents of trace 1-octanol and nonanal of real orange peel samples were quantified for the further method validation with satisfactory recoveries of 106.5 and 120.5%, respectively. This work proposed a sensitive, rapid, reliable and convenient analytical method for the potential study of trace and small molecular

  10. Preparation and evaluation of a novel molecularly imprinted polymer coating for selective extraction of indomethacin from biological samples by electrochemically controlled in-tube solid phase microextraction

    Energy Technology Data Exchange (ETDEWEB)

    Asiabi, Hamid [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Yamini, Yadollah, E-mail: yyamini@modares.ac.ir [Department of Chemistry, Tarbiat Modares University, P.O. Box 14115-175, Tehran (Iran, Islamic Republic of); Seidi, Shahram; Ghahramanifard, Fazel [Department of Analytical Chemistry, Faculty of Chemistry, K.N. Toosi University of Technology, Tehran (Iran, Islamic Republic of)

    2016-03-24

    In the present work, an automated on-line electrochemically controlled in-tube solid-phase microextraction (EC-in-tube SPME) coupled with HPLC-UV was developed for the selective extraction and preconcentration of indomethacin as a model analyte in biological samples. Applying an electrical potential can improve the extraction efficiency and provide more convenient manipulation of different properties of the extraction system including selectivity, clean-up, rate, and efficiency. For more enhancement of the selectivity and applicability of this method, a novel molecularly imprinted polymer coated tube was prepared and applied for extraction of indomethacin. For this purpose, nanostructured copolymer coating consisting of polypyrrole doped with ethylene glycol dimethacrylate was prepared on the inner surface of a stainless-steel tube by electrochemical synthesis. The characteristics and application of the tubes were investigated. Electron microscopy provided a cross linked porous surface and the average thickness of the MIP coating was 45 μm. Compared with the non-imprinted polymer coated tubes, the special selectivity for indomethacin was discovered with the molecularly imprinted coated tube. Moreover, stable and reproducible responses were obtained without being considerably influenced by interferences commonly existing in biological samples. Under the optimal conditions, the limits of detection were in the range of 0.07–2.0 μg L{sup −1} in different matrices. This method showed good linearity for indomethacin in the range of 0.1–200 μg L{sup −1}, with coefficients of determination better than 0.996. The inter- and intra-assay precisions (RSD%, n = 3) were respectively in the range of 3.5–8.4% and 2.3–7.6% at three concentration levels of 7, 70 and 150 μg L{sup −1}. The results showed that the proposed method can be successfully applied for selective analysis of indomethacin in biological samples. - Graphical abstract: An automated on

  11. Salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in high salinity and biological samples.

    Science.gov (United States)

    Niu, Zongliang; Yu, Chunwei; He, Xiaowen; Zhang, Jun; Wen, Yingying

    2017-09-05

    A salting-out assisted liquid-liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4mL of salting-out solution with pH=4 and the sample pH=3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5-5000ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5-60.6ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC-MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. "Collection of a lifetime: a practical approach to developing a longitudinal collection of women's healthcare biological samples".

    Science.gov (United States)

    Santillan, Mark K; Leslie, Kimberly K; Hamilton, Wendy S; Boese, Brenda J; Ahuja, Monika; Hunter, Stephen K; Santillan, Donna A

    2014-08-01

    The objective is to develop a biorepository of samples that represent all stages of a women's life. Importantly, our goal is to collect longitudinal physical specimens as well as the associated short and long-term clinical information. The Women's Health Tissue Repository was established to encompass four tissue banks: Well Women Tissue Bank, Reproductive Endocrinology and Infertility Tissue Bank, Maternal Fetal Tissue Bank, and the long-established Gynecologic Malignancies Tissue Bank. Based on their health status, women being seen in Women's Health at the University of Iowa are recruited to contribute samples and grant access to their electronic medical record to the biorepository. Samples are coded, processed, and stored for use by investigators. The Maternal Fetal Tissue Bank was the first expansion of our department's biobanking efforts. Approximately 75% of the women approached consent to participate in the Maternal Fetal Tissue Bank. Enrollment has steadily increased. Samples have been used for over 20 projects in the first 3 years and are critical to 7 funded grants and 3 patent applications. Patient samples with corresponding clinical data are initially important to women's health research. Our model demonstrates that many research projects by faculty, fellows, and residents have benefited from the existence of the Women's Health Tissue Repository. While challenging to achieve, longitudinal sampling allows for the greatest opportunity to study normal and pathological changes throughout all phases of a women's life, including pregnancy. This bank facilitates and accelerates the development of novel research, technologies, and possible therapeutic options in women's health. The establishment of more longitudinal biorepositories based on our model would enhance women's health research. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

  13. Towards tender X-rays with Zernike phase-contrast imaging of biological samples at 50 nm resolution.

    Science.gov (United States)

    Vartiainen, Ismo; Warmer, Martin; Goeries, Dennis; Herker, Eva; Reimer, Rudolph; David, Christian; Meents, Alke

    2014-07-01

    X-ray microscopy is a commonly used method especially in material science application, where the large penetration depth of X-rays is necessary for three-dimensional structural studies of thick specimens with high-Z elements. In this paper it is shown that full-field X-ray microscopy at 6.2 keV can be utilized for imaging of biological specimens with high resolution. A full-field Zernike phase-contrast microscope based on diffractive optics is used to study lipid droplet formation in hepatoma cells. It is shown that the contrast of the images is comparable with that of electron microscopy, and even better contrast at tender X-ray energies between 2.5 keV and 4 keV is expected.

  14. Evaluating the biological potential in samples returned from planetary satellites and small solar system bodies: framework for decision making

    National Research Council Canada - National Science Library

    National Research Council Staff; Space Studies Board; Division on Engineering and Physical Sciences; National Research Council; National Academy of Sciences

    ... from Planetary Satellites and Small Solar System Bodies Framework for Decision Making Task Group on Sample Return from Small Solar System Bodies Space Studies Board Commission on Physical Sciences, Mathematics, and Applications National Research Council NATIONAL ACADEMY PRESS Washington, D.C. 1998 i Copyrightthe true use are Please breaks...

  15. Public views on the donation and use of human biological samples in biomedical research: a mixed methods study.

    Science.gov (United States)

    Lewis, Celine; Clotworthy, Margaret; Hilton, Shona; Magee, Caroline; Robertson, Mark J; Stubbins, Lesley J; Corfield, Julie

    2013-08-07

    A mixed methods study exploring the UK general public's willingness to donate human biosamples (HBSs) for biomedical research. Cross-sectional focus groups followed by an online survey. Twelve focus groups (81 participants) selectively sampled to reflect a range of demographic groups; 1110 survey responders recruited through a stratified sampling method with quotas set on sex, age, geographical location, socioeconomic group and ethnicity. (1) Identify participants' willingness to donate HBSs for biomedical research, (2) explore acceptability towards donating different types of HBSs in various settings and (3) explore preferences regarding use and access to HBSs. 87% of survey participants thought donation of HBSs was important and 75% wanted to be asked to donate in general. Responders who self-reported having some or good knowledge of the medical research process were significantly more likely to want to donate (pfamily members might benefit. The most controversial types of HBSs to donate included: brain post mortem (29% would donate), eyes post mortem (35%), embryos (44%), spare eggs (48%) and sperm (58%). Regarding the use of samples, there were concerns over animal research (34%), research conducted outside the UK (35%), and research conducted by pharmaceutical companies (56%), although education and discussion were found to alleviate such concerns. There is a high level of public support and willingness to donate HBSs for biomedical research. Underlying concerns exist regarding the use of certain types of HBSs and conditions under which they are used. Improved education and more controlled forms of consent for sensitive samples may mitigate such concerns.

  16. Solid-phase microextraction for gas chromatographic/mass spectrometric analysis of dimethoate in human biological samples.

    Science.gov (United States)

    Gallardo, E; Barroso, M; Margalho, C; Cruz, A; Vieira, D N; López-Rivadulla, M

    2006-01-01

    A new, simple and rapid procedure for the determination of dimethoate in urine and blood samples was developed using direct immersion solid-phase microextraction and gas chromatography/mass spectrometry. This technique required only 0.1 mL of sample, and ethion was used as internal standard. Two types of coated fibre were compared (100 microm polydimethylsiloxane, and 65 microm Carbowax/divinylbenzene). Other parameters, such as extraction temperature, adsorption and desorption time, salt addition, agitation and pH, were optimized to enhance the sensitivity of the method. Limits of detection (LODs) and quantitation (LOQs) were 50 and 100 ng/mL for urine and 200 and 500 ng/mL for blood, respectively. The method was found to be linear between the LOQ and 40 microg/mL for urine, and between the LOQ and 50 microg/mL for blood, with correlation coefficients ranging from 0.9923-0.9996. Precision (intra- and interday) and accuracy were in conformity with the criteria normally accepted in bioanalytical method validation. The mean absolute recoveries of dimethoate were 1.24 and 0.50% for urine and blood, respectively. Because of its simplicity and the fact that small volumes of sample are used, the described method can be successfully used in the diagnosis of poisoning by this pesticide, namely in those situations where the sample volume is limited, as frequently occurs in forensic toxicology. Copyright 2006 John Wiley & Sons, Ltd.

  17. Evaluating the biological potential in samples returned from planetary satellites and small solar system bodies: framework for decision making

    National Research Council Canada - National Science Library

    National Research Council Staff

    1998-01-01

    ... from Planetary Satellites and Small Solar System Bodies Framework for Decision Making Task Group on Sample Return from Small Solar System Bodies Space Studies Board Commission on Physical Sciences, Mathematics, and Applications National Research Council NATIONAL ACADEMY PRESS Washington, D.C. 1998 i Copyrightthe true use are Please breaks...

  18. Applied research and development of neutron activation analysis - The study on human health and environment by neutron activation analysis of biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Seung Yeon; Yoo, Jong Ik; Lee, Jae Kwang; Lee, Sung Jun; Lee, Sang Sun; Jeon, Ki Hong; Na, Kyung Won; Kang, Sang Hun [Yonsei University, Seoul (Korea)

    2000-04-01

    With the development of the precise quantitative analytical method for the analysis of trace elements in the various biological samples such as hair and food, evaluation in view of health and environment to the trace elements in various sources which can be introduced inside human body was done. The trace elemental distribution in Korean total diet and representative food stuff was identified first. With the project the elemental distributions in supplemental healthy food and Korean and Chinese origin oriental medicine were identified. The amount of trace elements ingested with the hair analysis of oriental medicine takers were also estimated. The amounts of trace elements inhaled with the analysis of foundry air, blood and hair of foundry workers were also estimated. The basic estimation method in view of health and environment with the neutron activation analysis of biological samples such as foods and hair was established with the result. Nationwide usage system of the NAA facility in Hanaro in many different and important areas of biological area can be initiated with the results. The output of the project can support public heath, environment, and medical research area. The results can be applied for the process of micronutrients enhanced health food production and for the health safety and health status enhancement with the additional necessary data expansion and the development of various evaluation technique. 19 refs., 7 figs., 23 tabs. (Author)

  19. Ion-Exchange Sample Displacement Chromatography as a Method for Fast and Simple Isolation of Low- and High-Abundance Proteins from Complex Biological Mixtures

    Directory of Open Access Journals (Sweden)

    Martina Srajer Gajdosik

    2014-01-01

    Full Text Available Sample displacement chromatography (SDC in reversed phase and ion-exchange modes was introduced at the end of 1980s. This chromatographic method was first used for preparative purification of synthetic peptides, and subsequently adapted for protein fractionation, mainly in anion-exchange mode. In the past few years, SDC has been successfully used for enrichment of low- and medium-abundance proteins from complex biological fluids on both monolithic and bulk chromatographic supports. If aqueous mobile phase is used with the application of mild chromatographic conditions, isolated proteins are not denatured and can also keep their biological activity. In this paper, the use of SDC in anion-exchange mode on a high-capacity chromatographic resin for separation of proteins from complex biological mixtures such as human plasma is demonstrated. By use of three and more columns coupled in series during sample application, and subsequent parallel elution of detached columns, additional separation of bound proteins was achieved. Highly enriched human serum albumin fraction and a number of physiologically active medium- and low-abundance proteins could be fractionated and detected by electrospray ionization tandem mass spectrometry (ESI-MS/MS and matrix assisted laser desorption/ionization time-of-flight tandem mass spectrometry (MALDI-TOF/TOF-MS. The use of the aforementioned columns that can be sanitized with 1 M sodium hydroxide for further application of SDC in biotechnology and food technology was discussed.

  20. Use of Instrumental Neutron Activation Analysis for Determination of Some Trace Elements of Biological Importance in Different Jute(Corchorus Capsularis) Seed Samples

    International Nuclear Information System (INIS)

    Metwally, E.; Abd-El-Khalik, H.; El-Sweify, F.H.; El-Sweify, A.H.H.

    2004-01-01

    Instrumental neutron activation analysis technique was used to determine some trace elements in seeds of jute (corchorus capsularis). The seed samples were obtained from Agricultural Research Center (ARC), Giza, (EG). The analyzed seed samples were produced from cultivation of three different strains, namely: St. DC 1105, st. JRC 7447 and St. PADMA. These strains were imported from Bangladesh. The jute plant was cultivated in sandy soil in Ismailaya research station farm at may on two seasons 1999 and 2000. The plant was irrigated with water from Ismailaya canal. The study was carried out to compare the influence of applying different kinds of fertilizers of different rates, i.e. mineral fertilizer and biofertilizer, on the uptake of some biologically important trace elements and to determine their concentration in the analyzed jute seed samples. These elements were; Co,Cr,Fe,Zn and others eight elements were analyzed quantitatively

  1. Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for determination of three antifungal drugs in water and biological samples.

    Science.gov (United States)

    Ezoddin, Maryam; Shojaie, Mehran; Abdi, Khosrou; Karimi, Mohammad Ali

    2017-03-01

    A novel ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet (UAAD-LLM-SFO) followed by HPLC-UV detection was developed for the analysis of three antifungal drugs in water and biological samples. In this method, 1-dodecanol was used as the extraction solvent. The emulsion was rapidly formed by pulling in and pushing out the mixture of sample solution and extraction solvent for 5 times repeatedly using a 10-mL glass syringe while sonication was performed. Therefore, an organic dispersive solvent required in common microextraction methods was not used in the proposed method. After dispersing, an aliquot of acetonitrile was introduced as a demulsifier solvent into the sample solution to separate two phases. Therefore, some additional steps, such as the centrifugation, ultrasonication, or agitation of the sample solution, are not needed. Parameters influencing the extraction recovery were investigated. The proposed method showed a good linearity for the three antifungal drugs studied with the correlation coefficients (R 2  > 0.9995). The limits of detection (LODs) and the limits of the quantification (LOQs) were between 0.01-0.03 μg L -1 and 0.03-0.08 μg L -1 , respectively. The preconcentration factors (PFs) were in the range of 107-116, respectively. The precisions, as the relative standard deviations (RSDs) (n = 5), for inter-day and intra-day analysis were in the range of 2.1-4.5% and 6.5-8.5%, respectively. This method was successfully applied to determine the three antifungal drugs in tap water and biological samples. The recoveries of antifungal drugs in these samples were 92.4-98.5%. Graphical abstract Ultrasound-air-assisted demulsified liquid-liquid microextraction by solidification of a floating organic droplet for the analysis of three antifungal drugs prior HPLC-UV.

  2. Method Performance of Total Mercury (Hg) Testing in the Biological Samples by Using Cold Vapour Atomic Absorption Spectrophotometer (CV-AAS)

    International Nuclear Information System (INIS)

    Susanna TS; Samin

    2007-01-01

    Method performance (validation) of total mercury (Hg) testing in the biological samples by using cold vapour atomic absorption spectrophotometer (CV-AAS) has been done. The objective of this research is to know the method performance of CV-AAS as one of points for the accreditation testing of laboratory according IS0/IEC 17025-2005. The method performance covering limit of detection (LOD), accuracy, precision and bias. As a standard material used SRM Oyster Tissue 15660 from Winopal Forshung Germany, whereas the biological samples were human hair. In principle of mercury testing for solid samples using CV-AAS is dissolving this sample and standard with 10 mL HNO 3 supra pure into a closed quartz tube and heating at 150 °C for 4 hours. The concentration of mercury in each samples was determined at the condition of operation were stirring time (T 1 ) 70 seconds, delay time (T 2 ) 15 seconds, heating time (T 3 ) 13 seconds and cooling time (T 4 ) of 25 seconds. Mercury ion in samples are reduced with SnCl 2 10 % in H 2 SO 4 20 %, and then the vapour of mercury from reduction is passed in NaOH 20 % solution and aquatridest. The result of method performance were: limit of detection (LOD) = 0.085 ng, accuracy 99.70 %, precision (RSD) = 1.64 % and bias = 0.30 %. From the validation result showed that the content of mercury total was in the range of certified values. The total mercury content (Hg) in human hair were varied from 406.93 - 699.07 ppb. (author)

  3. Grafting of allylimidazole and n-vinylcaprolactam as a thermosensitive polymer onto magnetic nano-particles for the extraction and determination of celecoxib in biological samples.

    Science.gov (United States)

    Morovati, Atefeh; Ahmad Panahi, Homayon; Yazdani, Farzaneh

    2016-11-20

    In this research, a novel method is reported for the surface grafting of n-vinylcaprolactam as a thermosensitive agent and allylimidazole with affinity toward celecoxib onto magnetic nano-particles. The grafted nano-particles were characterized by Fourier transform infrared spectroscopy, elemental analysis, and thermogravimetric analysis. The surface morphology was studied using Scanning Electron Microscopy. The resulting grafted nano-particles were used for the determination of trace celecoxib in biological human fluids and pharmaceutical samples. The profile of celecoxib uptake by the modified magnetic nano-particles indicated good accessibility of the active sites in the grafted copolymer. It was found that the adsorption behavior could be fitted by the Langmuir adsorption isotherm model. Solid phase extraction for biological fluids such as urine and serum were investigated. In this study, urine extraction recovery of more than 95% was obtained. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Context matters: volunteer bias, small sample size, and the value of comparison groups in the assessment of research-based undergraduate introductory biology lab courses.

    Science.gov (United States)

    Brownell, Sara E; Kloser, Matthew J; Fukami, Tadashi; Shavelson, Richard J

    2013-01-01

    The shift from cookbook to authentic research-based lab courses in undergraduate biology necessitates the need for evaluation and assessment of these novel courses. Although the biology education community has made progress in this area, it is important that we interpret the effectiveness of these courses with caution and remain mindful of inherent limitations to our study designs that may impact internal and external validity. The specific context of a research study can have a dramatic impact on the conclusions. We present a case study of our own three-year investigation of the impact of a research-based introductory lab course, highlighting how volunteer students, a lack of a comparison group, and small sample sizes can be limitations of a study design that can affect the interpretation of the effectiveness of a course.

  5. [Logistics of collection and transportation of biological samples and the organization of the central laboratory in the ELSA-Brasil].

    Science.gov (United States)

    Fedeli, Ligia G; Vidigal, Pedro G; Leite, Claudia Mendes; Castilhos, Cristina D; Pimentel, Robércia Anjos; Maniero, Viviane C; Mill, Jose Geraldo; Lotufo, Paulo A; Pereira, Alexandre C; Bensenor, Isabela M

    2013-06-01

    The ELSA (Estudo Longitudinal de Saúde do Adulto - Brazilian Longitudinal Study for Adult Health) is a multicenter cohort study which aims at the identification of risk factors associated with type 2 diabetes and cardiovascular diseases in the Brazilian population. The paper describes the strategies for the collection, processing, transportation, and quality control of blood and urine tests in the ELSA. The study decided to centralize the tests at one single laboratory. The processing of the samples was performed at the local laboratories, reducing the weight of the material to be transported, and diminishing the costs of transportation to the central laboratory at the Universidade de São Paulo Hospital. The study included tests for the evaluation of diabetes, insulin resistance, dyslipidemia, electrolyte abnormalities, thyroid hormones, uric acid, hepatic enzyme abnormalities, inflammation, and total blood cell count. In addition, leukocyte DNA, urine, plasma and serum samples were stored. The central laboratory performed approximately 375,000 tests.

  6. Quantification of chlorine in zirconium oxide and biological samples by instrumental NAA utilizing PCF of Dhruva reactor

    International Nuclear Information System (INIS)

    Shinde, Amol D.; Reddy, A.V.R.; Acharya, R.; Balaji Rao, Y.

    2012-01-01

    Recently studies on chlorine contents in various samples are being pursued due to its corrosive nature. Chlorine present at trace level in various finished products as well as powder is used as a raw material for production of different types of zircaloys used as structural materials in nuclear technology. As a part of quality assurance program, it is necessary to quantify chlorine accurately with suitable and simple technique. In the present work we have applied instrumental neutron activation analysis (INAA) utilizing its short-lived activation product ( 38 Cl, 37 min, 1642 and 2168 keV) for its estimation. Pneumatic Carrier Facility (PCF) of Dhruva reactor, BARC was used sample irradiation of zirconium oxide dry powder, synthetic wax and IAEA RMs 1515 (Apple leaves) and Lichen 336. (author)

  7. Surfactant assisted pulsed two-phase electromembrane extraction followed by GC analysis for quantification of basic drugs in biological samples.

    Science.gov (United States)

    Zahedi, Pegah; Davarani, Saied Saeed Hosseiny; Moazami, Hamid Reza; Nojavan, Saeed

    2016-01-05

    In this work, a simple and efficient surfactant assisted pulsed two-phase electromembrane extraction (SA-PEME) procedure combined with gas chromatography (GC) has been developed for the determination of alfentanil, sufentanil and methadone in various samples. It has been found that the addition of anionic surfactant causes the accumulation of the cationic analytes at the SLM/solution interface resulting in an easier transfer of the analytes into the organic phase. The method was accomplished with 1-octanol as the acceptor phase and supported liquid membrane (SLM) by means of an 80 V pulsed electrical driving force and the extraction time of 20 min. The model analytes were extracted from 3.0 mL sample solution (pH 4.0) containing 0.02% w/v surfactant (sodium dodecyl sulfate). The duty cycle of 92% and frequency of 0.357 Hz gave the best performance. Extraction recoveries in the range of 70.5-95.2% and satisfactory repeatability (7.6samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  8. Liquid scintillation based quantitative measurement of dual radioisotopes (3H and 45Ca) in biological samples for bone remodeling studies.

    Science.gov (United States)

    Hui, Susanta K; Sharma, M; Bhattacharyya, M H

    2012-01-01

    Acute and prolonged bone complications associated with radiation and chemotherapy in cancer survivors underscore the importance of establishing a laboratory-based complementary dual-isotope tool to evaluate short- as well as long-term bone remodeling in an in vivo model. To address this need, a liquid scintillation dual-label method was investigated using different scintillation cocktails for quantitative measurement of (3)H-tetracycline ((3)H-TC) and (45)Ca as markers of bone turnover in mice. Individual samples were prepared over a wide range of known (45)Ca/(3)H activity ratios. Results showed that (45)Ca/(3)H activity ratios determined experimentally by the dual-label method were comparable to the known activity ratios (percentage difference ∼2%), but large variations were found in samples with (45)Ca/(3)H activity ratios in range of 2-10 (percentage difference ∼20-30%). Urine and fecal samples from mice administered with both (3)H-TC and (45)Ca were analyzed with the dual-label method. Positive correlations between (3)H and (45)Ca in urine (R=0.93) and feces (R=0.83) indicate that (3)H-TC and (45)Ca can be interchangeably used to monitor longitudinal in vivo skeletal remodeling. Copyright © 2011 Elsevier Ltd. All rights reserved.

  9. Biological Sampling and Analysis in Sinclair and Dyes Inlets, Washington: Chemical Analyses for 2007 Puget Sound Biota Study

    Energy Technology Data Exchange (ETDEWEB)

    Brandenberger, Jill M.; Suslick, Carolynn R.; Johnston, Robert K.

    2008-10-09

    Evaluating spatial and temporal trends in contaminant residues in Puget Sound fish and macroinvertebrates are the objectives of the Puget Sound Ambient Monitoring Program (PSAMP). In a cooperative effort between the ENVironmental inVESTment group (ENVVEST) and Washington State Department of Fish and Wildlife, additional biota samples were collected during the 2007 PSAMP biota survey and analyzed for chemical residues and stable isotopes of carbon (δ13C) and nitrogen (δ15N). Approximately three specimens of each species collected from Sinclair Inlet, Georgia Basin, and reference locations in Puget Sound were selected for whole body chemical analysis. The muscle tissue of specimens selected for chemical analyses were also analyzed for δ13C and δ15N to provide information on relative trophic level and food sources. This data report summarizes the chemical residues for the 2007 PSAMP fish and macro-invertebrate samples. In addition, six Spiny Dogfish (Squalus acanthias) samples were necropsied to evaluate chemical residue of various parts of the fish (digestive tract, liver, embryo, muscle tissue), as well as, a weight proportional whole body composite (WBWC). Whole organisms were homogenized and analyzed for silver, arsenic, cadmium, chromium, copper, nickel, lead, zinc, mercury, 19 polychlorinated biphenyl (PCB) congeners, PCB homologues, percent moisture, percent lipids, δ13C, and δ15N.

  10. Liquid scintillation based quantitative measurement of dual radioisotopes (3H and 45Ca) in biological samples for bone remodeling studies

    Science.gov (United States)

    Hui, Susanta K; Sharma, M; Bhattacharyya, M H

    2011-01-01

    Acute and prolonged bone complications associated with radiation and chemotherapy in cancer survivors underscore the importance of establishing a laboratory-based complementary dual-isotope tool to evaluate short- as well as long-term bone remodeling in an in vivo model. To address this need, a liquid scintillation dual-label method was investigated using different scintillation cocktails for quantitative measurement of 3H-tetracycline (3H-TC) and 45Ca as markers of bone turnover in mice. Individual samples were prepared over a wide range of known 45Ca/3H activity ratios. Results showed that 45Ca/3H activity ratios determined experimentally by the dual-label method were comparable to the known activity ratios (percentage difference ~2%), but large variations were found in samples with 45Ca/3H activity ratios in range of 2–10 (percentage difference ~ 20–30%). Urine and fecal samples from mice administered with both 3H-TC and 45Ca were analyzed with the dual-label method. Positive correlations between 3H and 45Ca in urine (R = 0.93) and feces (R = 0.83) indicate that 3H-TC and 45Ca can be interchangeably used to monitor longitudinal in vivo skeletal remodeling. PMID:21900015

  11. An enzymatic method of analysis for GDP-L-fucose in biological samples, involving high-performance liquid chromatography.

    Science.gov (United States)

    Noda, Katsuhisa; Miyoshi, Eiji; Nakahara, Susumu; Ihara, Hideyuki; Gao, Cong Xiao; Honke, Koichi; Yanagidani, Shusaku; Sasaki, Yutaka; Kasahara, Akinori; Hori, Masatsugu; Hayashi, Norio; Taniguchi, Naoyuki

    2002-11-01

    To investigate the biological significance of GDP-L-fucose, we established a unique method for the determination of GDP-L-fucose levels in microsomal fractions, using an HPLC assay of alpha 1-6-fucosyltransferase (alpha1-6-FucT), an enzyme that catalyzes the synthesis of core fucosylation in N-glycans. A microsomal protein and a large excess of fluorescence-labeled synthetic oligosaccharide (a substrate) were incubated with a large excess of alpha1-6-FucT. The fluorescent intensity of the fucosylated reaction product, which was analyzed by isocratic reverse phase HPLC, was proportional to the level of GDP-L-fucose in the microsomal fractions over the range 0.20-10 pmol. This assay is applicable to the determination of the GDP-L-fucose content in various cancer cell lines as well as rat liver and would be useful in developing a better understanding of the fucosylation potential of such cells and tissues.

  12. Synchrotron radiation. 4. Analyses of biological samples using synchrotron radiation. 3. Research on radiation damage to DNA using synchrotron radiation

    International Nuclear Information System (INIS)

    Takakura, Kaoru

    1998-01-01

    This review described how the synchrotron radiation (SR) is used to solve problems unknown hitherto in radiation biology. Historically, the target substance of UV light in bacterial death was suggested to be nucleic acid in 1930. Researches on the radiation damage to DNA were begun at around 1960 and have mainly used UV light, X-ray and γray. Soft X-ray and vacuum UV whose energy covering from several eV to scores of keV have not been used since UV and X-ray lack the energy of this range. This is one of reasons why detailed process leading to radiation-induced death, carcinogenicity and mutation has not been known hitherto. RS possesses wide range of energy, i.e., from UV to hard X-ray, of high intensity, which is helpful for studying the unknown problems. The RS studies were begun in nineteen-seventies. Those include the action spectrum studies and atomic target studies. In the former, the course of the effect, e.g., the mechanism of DNA double strand breakage, can be elucidated. In the latter, photon of known energy can be irradiated to the specified atom like phosphorus in DNA which elucidating the precise physicochemical process of the breakage. Use of RS in these studies is thought still meaningful in future. (K.H.) 62 refs

  13. Differential pulse polarographic determination of trace antimony in standard biological samples after preconcentration using 2-nitroso-1-naphthol-4-sulfonic acid

    International Nuclear Information System (INIS)

    Taher, M. A.

    2003-01-01

    A highly selective, rapid and economical differential polarographic method has been developed for the determination of trace amounts of antimony in various standard alloys and biological samples after of its 2-naphthol-4 sulfonic acid tetradecyl dimethylbenzylammonium chloride on microcrystalline naphthalene in the ph range of 7.5-11.0. After filtration, the solid mass is shaken with 8-10 ml of 1 M hydrochloric acid (with preconcentration factor of 10) and antimony is determined by differential pulse polarography. Antimony can alternatively be quantitatively absorbed on 2-nitroso-1-naphthol-4-sulfonic acid tetradecyl dimethylbenzylammonium-naphthalene absorbed packed in a column (with preconcentration factor of 30) and determined similarly. In this case, 1.5 μg of antimony can be concentrated in a column from 300 ml of aqueous sample, where its concentration is as low as 5 ng/ml. Characterization of the electro active process included an examination of the degree of reversibility. The results show that the irreversibility of antimony. Various parameters such as the effect of ph, volume of aqueous phase, HCl concentration, reagent concentration, naphthalene concentration, shaking time and interference of a number of metal ions on the determination of antimony have been studied in detail to optimize the conditions for determination in standard alloys and standard biological samples

  14. Systematic approach to optimize a pretreatment method for ultrasensitive liquid chromatography with tandem mass spectrometry analysis of multiple target compounds in biological samples.

    Science.gov (United States)

    Togashi, Kazutaka; Mutaguchi, Kuninori; Komuro, Setsuko; Kataoka, Makoto; Yamazaki, Hiroshi; Yamashita, Shinji

    2016-08-01

    In current approaches for new drug development, highly sensitive and robust analytical methods for the determination of test compounds in biological samples are essential. These analytical methods should be optimized for every target compound. However, for biological samples that contain multiple compounds as new drug candidates obtained by cassette dosing tests, it would be preferable to develop a single method that allows the determination of all compounds at once. This study aims to establish a systematic approach that enables a selection of the most appropriate pretreatment method for multiple target compounds without the use of their chemical information. We investigated the retention times of 27 known compounds under different mobile phase conditions and determined the required pretreatment of human plasma samples using several solid-phase and liquid-liquid extractions. From the relationship between retention time and recovery in a principal component analysis, appropriate pretreatments were categorized into several types. Based on the category, we have optimized a pretreatment method for the identification of three calcium channel blockers in human plasma. Plasma concentrations of these drugs in a cassette-dose clinical study at microdose level were successfully determined with a lower limit of quantitation of 0.2 pg/mL for diltiazem, 1 pg/mL for nicardipine, and 2 pg/mL for nifedipine. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  15. Application of direct solid sample analysis for the determination of chlorine in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Santos de Gois, Jefferson; Pereira, Éderson R. [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); Welz, Bernhard [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil); Borges, Daniel L.G., E-mail: daniel.borges@ufsc.br [Departamento de Química, Universidade Federal de Santa Catarina, 88040-970 Florianópolis, SC (Brazil); INCT de Energia e Ambiente do CNPq (Brazil)

    2015-03-01

    This work describes a methodology developed to carry out Cl determination in biological materials using electrothermal vaporization inductively coupled plasma mass spectrometry and direct solid sample analysis. The solid samples were directly weighed into graphite ‘cups’ and inserted into the graphite furnace. The RF power and the carrier gas flow rate were optimized at 1300 W and 0.7 L min{sup −1}, respectively. Calibration could be carried out using aqueous standard solutions with pre-dried modifiers (Pd + Nd or Pd + Ca) or using solid certified reference materials with the same pre-dried modifiers or without the use of modifiers. The limit of quantification was determined as 5 μg g{sup −1} under optimized conditions and the Cl concentration was determined in five certified reference materials with certified concentrations for Cl, in addition to three certified reference materials, for which certified values for Cl were unavailable; in the latter case, the results were compared with those obtained using high-resolution continuum source molecular absorption spectrometry. Good agreement at a 95% statistical confidence level was achieved between determined and certified or reference values. - Highlights: • Direct determination of chlorine in solid biological materials is described for the first time using ICP-MS. • Calibration against aqueous standards is feasible. • The method is accurate and sensitive, regardless of the composition of the solid sample.

  16. Applications of Isotope Ratio Mass Spectrometry in Sports Drug Testing Accounting for Isotope Fractionation in Analysis of Biological Samples.

    Science.gov (United States)

    Piper, Thomas; Thevis, Mario

    2017-01-01

    The misuse of anabolic-androgenic steroids (AAS) in sports aiming at enhancing athletic performance has been a challenging matter for doping control laboratories for decades. While the presence of a xenobiotic AAS or its metabolite(s) in human urine immediately represents an antidoping rule violation, the detection of the misuse of endogenous steroids such as testosterone necessitates comparably complex procedures. Concentration thresholds and diagnostic analyte ratios computed from urinary steroid concentrations of, e.g., testosterone and epitestosterone have aided identifying suspicious doping control samples in the past. These ratios can however also be affected by confounding factors and are therefore not sufficient to prove illicit steroid administrations. Here, carbon and, in rare cases, hydrogen isotope ratio mass spectrometry (IRMS) has become an indispensable tool. Importantly, the isotopic signatures of pharmaceutical steroid preparations commonly differ slightly but significantly from those found with endogenously produced steroids. By comparing the isotope ratios of endogenous reference compounds like pregnanediol to that of testosterone and its metabolites, the unambiguous identification of the urinary steroids' origin is accomplished. Due to the complex urinary matrix, several steps in sample preparation are inevitable as pure analyte peaks are a prerequisite for valid IRMS determinations. The sample cleanup encompasses steps such as solid phase or liquid-liquid extraction that are presumably not accompanied by isotopic fractionation processes, as well as more critical steps like enzymatic hydrolysis, high-performance liquid chromatography fractionation, and derivatization of analytes. In order to exclude any bias of the analytical results, each step of the analytical procedure is optimized and validated to exclude, or at least result in constant, isotopic fractionation. These efforts are explained in detail. © 2017 Elsevier Inc. All rights reserved.

  17. A nested-PCR strategy for molecular diagnosis of mollicutes in uncultured biological samples from cows with vulvovaginitis.

    Science.gov (United States)

    Voltarelli, Daniele Cristina; de Alcântara, Brígida Kussumoto; Lunardi, Michele; Alfieri, Alice Fernandes; de Arruda Leme, Raquel; Alfieri, Amauri Alcindo

    2018-01-01

    Bacteria classified in Mycoplasma (M. bovis and M. bovigenitalium) and Ureaplasma (U. diversum) genera are associated with granular vulvovaginitis that affect heifers and cows at reproductive age. The traditional means for detection and speciation of mollicutes from clinical samples have been culture and serology. However, challenges experienced with these laboratory methods have hampered assessment of their impact in pathogenesis and epidemiology in cattle worldwide. The aim of this study was to develop a PCR strategy to detect and primarily discriminate between the main species of mollicutes associated with reproductive disorders of cattle in uncultured clinical samples. In order to amplify the 16S-23S rRNA internal transcribed spacer region of the genome, a consensual and species-specific nested-PCR assay was developed to identify and discriminate between main species of mollicutes. In addition, 31 vaginal swab samples from dairy and beef affected cows were investigated. This nested-PCR strategy was successfully employed in the diagnosis of single and mixed mollicute infections of diseased cows from cattle herds from Brazil. The developed system enabled the rapid and unambiguous identification of the main mollicute species known to be associated with this cattle reproductive disorder through differential amplification of partial fragments of the ITS region of mollicute genomes. The development of rapid and sensitive tools for mollicute detection and discrimination without the need for previous cultures or sequencing of PCR products is a high priority for accurate diagnosis in animal health. Therefore, the PCR strategy described herein may be helpful for diagnosis of this class of bacteria in genital swabs submitted to veterinary diagnostic laboratories, not demanding expertise in mycoplasma culture and identification. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Minimization of the blank values in the neutron activation analysis of biological samples considering the whole procedure

    International Nuclear Information System (INIS)

    Lux, F.; Bereznai, T.; Trebert Haeberlin, S.

    1987-01-01

    During the determination of trace element contents of animal tissue by neutron activation analysis in the course of structure-activity relationship studies on platinum containing cancer drugs and wound healing the authors tried to minimize the blank values that are caused by different sources of contamination during surgery, sampling and the activation analysis procedure. The following topics were investigated: abrasions from scalpels made of stainless steel, titanium or quartz, the type of surgery, the surface contaminations of the quartz ampoules, etc. The measures to be taken to reduce tha blank values are described. (author) 19 refs.; 4 tables

  19. Simultaneous determination of trace levels of ethylmercury and methylmercury in biological samples and vaccines using sodium tetra(n-propyl)borate as derivatizing agent

    Energy Technology Data Exchange (ETDEWEB)

    Gibicar, Darija; Logar, Martina; Horvat, Nusa; Horvat, Milena [Jozef Stefan Institute, Department of Environmental Sciences, Ljubljana (Slovenia); Marn-Pernat, Andreja; Ponikvar, Rafael [University Medical Centre, Department of Nephrology, Ljubljana (Slovenia)

    2007-05-15

    Because of increasing awareness of the potential neurotoxicity of even low levels of organomercury compounds, analytical techniques are required for determination of low concentrations of ethylmercury (EtHg) and methylmercury (MeHg) in biological samples. An accurate and sensitive method has been developed for simultaneous determination of methylmercury and ethylmercury in vaccines and biological samples. MeHg and EtHg were isolated by acid leaching (H{sub 2}SO{sub 4}-KBr-CuSO{sub 4}), extraction of MeHg and EtHg bromides into an organic solvent (CH{sub 2}Cl{sub 2}), then back-extraction into Milli-Q water. MeHg and EtHg bromides were derivatized with sodium tetrapropylborate (NaBPr{sub 4}), collected at room temperature on Tenax, separated by isothermal gas chromatography (GC), pyrolysed, and detected by cold-vapour atomic fluorescence spectrometry (CV AFS). The repeatability of results from the method was approximately 5-10% for EtHg and 5-15% for MeHg. Detection limits achieved were 0.01 ng g{sup -1} for EtHg and MeHg in blood, saliva, and vaccines and 5 ng g{sup -1} for EtHg and MeHg in hair. The method presented has been shown to be suitable for determination of background levels of these contaminants in biological samples and can be used in studies related to the health effects of mercury and its species in man. This work illustrates the possibility of using hair and blood as potential biomarkers of exposure to thiomersal. (orig.)

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

    Science.gov (United States)

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

    2011-11-01

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

  1. Simultaneous determination and validation of emtricitabine, rilpivirine and tenofovir from biological samples using LC and CE methods.

    Science.gov (United States)

    Gumustas, Mehmet; Caglayan, Mehmet Gokhan; Onur, Feyyaz; Ozkan, Sibel A

    2018-04-01

    A combination of antiretroviral agents is frequently used in effective treatment of the human immunodeficiency virus infection. In this study, two different separation methods are presented for the simultaneous determination of emtricitabine, rilpivirine and tenofovir from raw materials and urine samples. Developed liquid chromatography and capillary electrophoresis methods were thoroughly optimized for high analytical performances. Optimization of multiple variables at the same time by performing a minimum number of experiments was achieved by the Box-Behnken design, which is an experimental design in response surface methodology, in capillary electrophoresis. The results of the experimental design ensure minimum analysis time with well-separated analytes. Separation conditions, such as different stationary phases, pH level, organic modifiers and temperatures in liquid chromatography method, were also optimized. In particular, among stationary phases, the core-shell column especially enhanced the effectiveness of separation in liquid chromatography. Both methods were fully validated and applied to real samples. The main advantage of the developed methods is the separation of the drug combination in a short time with high efficiency and without any time-consuming steps. Copyright © 2017 John Wiley & Sons, Ltd.

  2. Simultaneous multi-species determination of trimethyllead, monomethylmercury and three butyltin compounds by species-specific isotope dilution GC-ICP-MS in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Poperechna, Nataliya; Heumann, Klaus G. [Johannes Gutenberg-University Mainz (Germany). Institute of Inorganic Chemistry and Analytical Chemistry

    2005-09-01

    An accurate and sensitive multi-species species-specific isotope dilution GC-ICP-MS method was developed for the simultaneous determination of trimethyllead (Me{sub 3}Pb{sup +}), monomethylmercury (MeHg{sup +}) and the three butyltin species Bu{sub 3}Sn{sup +}, Bu{sub 2}Sn{sup 2+}, and BuSn{sup 3+} in biological samples. The method was validated by three biological reference materials (CRM 477, mussel tissue certified for butyltins; CRM 463, tuna fish certified for MeHg{sup +}; DORM 2, dogfish muscle certified for MeHg{sup +}). Under certain conditions, and with minor modifications of the sample pretreatment procedure, this method could also be transferred to environmental samples such as sediments, as demonstrated by analyzing sediment reference material BCR 646 (freshwater sediment, certified for butyltins). The detection limits of the multi-species GC-ICP-IDMS method for biological samples were 1.4 ng g{sup -1} for MeHg{sup +}, 0.06 ng g{sup -1} for Me{sub 3}Pb{sup +}, 0.3 ng g{sup -1} for BuSn{sup 3+} and Bu{sub 3}Sn{sup +}, and 1.2 ng g{sup -1} for Bu{sub 2}Sn{sup 2+}. Because of the high relevance of these heavy metal alkyl species to the quality assurance of seafood, the method was also applied to corresponding samples purchased from a supermarket. The methylated lead fraction in these samples, correlated to total lead, varied over a broad range (from 0.01% to 7.6%). On the other hand, the MeHg{sup +} fraction was much higher, normally in the range of 80-100%. Considering that we may expect tighter legislative limitations on MeHg{sup +} levels in seafood in the future, we found the highest methylmercury contents (up to 10.6 {mu}g g{sup -1}) in two shark samples, an animal which is at the end of the marine food chain, whereas MeHg{sup +} contents of less than 0.2 {mu}g g{sup -1} were found in most other seafood samples; these results correlate with the idea that MeHg{sup +} is usually of biological origin in the marine environment. The concentration of

  3. Precision and accuracy in the quantitative analysis of biological samples by accelerator mass spectrometry: application in microdose absolute bioavailability studies.

    Science.gov (United States)

    Gao, Lan; Li, Jing; Kasserra, Claudia; Song, Qi; Arjomand, Ali; Hesk, David; Chowdhury, Swapan K

    2011-07-15

    Determination of the pharmacokinetics and absolute bioavailability of an experimental compound, SCH 900518, following a 89.7 nCi (100 μg) intravenous (iv) dose of (14)C-SCH 900518 2 h post 200 mg oral administration of nonradiolabeled SCH 900518 to six healthy male subjects has been described. The plasma concentration of SCH 900518 was measured using a validated LC-MS/MS system, and accelerator mass spectrometry (AMS) was used for quantitative plasma (14)C-SCH 900518 concentration determination. Calibration standards and quality controls were included for every batch of sample analysis by AMS to ensure acceptable quality of the assay. Plasma (14)C-SCH 900518 concentrations were derived from the regression function established from the calibration standards, rather than directly from isotopic ratios from AMS measurement. The precision and accuracy of quality controls and calibration standards met the requirements of bioanalytical guidance (U.S. Department of Health and Human Services, Food and Drug Administration, Center for Drug Evaluation and Research, Center for Veterinary Medicine. Guidance for Industry: Bioanalytical Method Validation (ucm070107), May 2001. http://www.fda.gov/downloads/Drugs/GuidanceCompilanceRegulatoryInformation/Guidances/ucm070107.pdf ). The AMS measurement had a linear response range from 0.0159 to 9.07 dpm/mL for plasma (14)C-SCH 900158 concentrations. The CV and accuracy were 3.4-8.5% and 94-108% (82-119% for the lower limit of quantitation (LLOQ)), respectively, with a correlation coefficient of 0.9998. The absolute bioavailability was calculated from the dose-normalized area under the curve of iv and oral doses after the plasma concentrations were plotted vs the sampling time post oral dose. The mean absolute bioavailability of SCH 900518 was 40.8% (range 16.8-60.6%). The typical accuracy and standard deviation in AMS quantitative analysis of drugs from human plasma samples have been reported for the first time, and the impact of these

  4. A forward mutation assay using ampicillin-resistance in Escherichia coli designed for investigating the mutagenicity of biological samples.

    Science.gov (United States)

    Bosworth, D; Crofton-Sleigh, C; Venitt, S

    1987-11-01

    The development of a bacterial mutation assay using forward mutation to ampicillin-resistance is described. It is a technically simple assay using Escherichia coli D494uvrB transformed with a multi-copy mutator plasmid pGW1700. Mutation is detected by an increase in the frequency of ampicillin-resistant colonies following treatment of bacteria with the test material during logarithmic growth. The determination of viable counts allows a correction factor to be applied to compensate for the effects of sample-induced growth enhancement or toxicity on the bacterial population. The assay has been tested with a range of reference mutagens. It is particularly sensitive to base-pair substitution mutagens, detecting these at doses equal to or less than those detected in the Salmonella/microsome assay or the SOS Chromotest. The assay also detects frameshift mutagens but with lower sensitivity than the Salmonella/microsome assay.

  5. One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples.

    Science.gov (United States)

    Sun, Jieping; Liang, Qionglin; Han, Qiang; Zhang, Xiaoqiong; Ding, Mingyu

    2015-01-01

    A novel magnetic graphene oxide nanocomposite was synthesized by one-step coprecipitation method and characterized by transmission electron microscopy, X-ray photoelectron spectroscopy and vibrating sample magnetometer. The nanocomposite beard many intriguing properties, including chemical stability, high adsorption capacity, and superparamagnetic. These properties evoked great interest and desire of its exploration in magnetic solid-phase extraction of heavy metal ions from complex samples. Several parameters effecting the analytical performance, such as the sample pH, amounts of adsorbent, sample volumes, elution volumes, and coexisting ions, had been investigated in detail. The adsorbed metal ions were easy eluted by controlling the pH condition and the materials could be reused more than 20 times. Under the optimized conditions, the limits of detection were 0.016, 0.046, 0.395, 0.038, 0.157 μg L(-1) for Co(2+), Ni(2+), Cu(2+), Cd(2+), and Pb(2+), respectively. The intra-day relative standard deviations (n=5) were in the range of 1.8-5.5% at 10 μg L(-1). The proposed method was successfully applied to biological sample analysis and got excellent recoveries in the range of 81-113% even the matrix was complex. Copyright © 2014 Elsevier B.V. All rights reserved.

  6. The Upgrade Programme for the Structural Biology beamlines at the European Synchrotron Radiation Facility – High throughput sample evaluation and automation

    International Nuclear Information System (INIS)

    Theveneau, P; Baker, R; Barrett, R; Beteva, A; Bowler, M W; Carpentier, P; Caserotto, H; Sanctis, D de; Dobias, F; Flot, D; Guijarro, M; Giraud, T; Lentini, M; Leonard, G A; Mattenet, M; McSweeney, S M; Morawe, C; Nurizzo, D; McCarthy, A A; Nanao, M

    2013-01-01

    Automation and advances in technology are the key elements in addressing the steadily increasing complexity of Macromolecular Crystallography (MX) experiments. Much of this complexity is due to the inter-and intra-crystal heterogeneity in diffraction quality often observed for crystals of multi-component macromolecular assemblies or membrane proteins. Such heterogeneity makes high-throughput sample evaluation an important and necessary tool for increasing the chances of a successful structure determination. The introduction at the ESRF of automatic sample changers in 2005 dramatically increased the number of samples that were tested for diffraction quality. This 'first generation' of automation, coupled with advances in software aimed at optimising data collection strategies in MX, resulted in a three-fold increase in the number of crystal structures elucidated per year using data collected at the ESRF. In addition, sample evaluation can be further complemented using small angle scattering experiments on the newly constructed bioSAXS facility on BM29 and the micro-spectroscopy facility (ID29S). The construction of a second generation of automated facilities on the MASSIF (Massively Automated Sample Screening Integrated Facility) beam lines will build on these advances and should provide a paradigm shift in how MX experiments are carried out which will benefit the entire Structural Biology community.

  7. Use of biomarkers to evaluate the effects of environmental stressors on Mytilus galloprovincialis sampled along the Moroccan coasts: Integrating biological and chemical data.

    Science.gov (United States)

    El Haimeur, Bouchra; Bouhallaoui, Mina; Zbiry, Mariama; Elkhiati, Najat; Talba, Sophia; Sforzini, Susanna; Viarengo, Aldo; Benhra, Ali

    2017-09-01

    A biomonitoring study using wild Mytilus galloprovincialis mussels sampled from six sites along the Moroccan coasts evaluated whether select biomarkers are suitable for identifying and quantifying pollution-induced stress syndrome in mussels. Lysosomal membrane stability was confirmed to be a highly sensitive biological parameter, and acetylcholinesterase activity was found a suitable biomarker of neurotoxicity. Metallothionein concentrations were in line with heavy metal concentrations detected in mussel tissues. However, malondialdehyde was not sensitive, suggesting the need for alternative biomarkers of oxidative stress. Three different approaches were used for biomarker and chemical data integration. The Integrated Biomarker Response (IBR) was suitable for classifying the stress response but did not allow to evaluate the level of stress in the organisms. The Mussel Expert System (MES) was suitable for ranking the biological effects of pollutants, also providing an indication of the evolution of the stress syndrome in the animals. Finally, the use of Principal Component Analysis (PCA) provided indication of the inorganic chemicals contributing to the detrimental biological effects. Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Characterization of medical and biological samples with a Talbot–Lau grating interferometer μXCT in comparison to reference methods

    Directory of Open Access Journals (Sweden)

    Christian Gusenbauer

    2016-11-01

    Full Text Available Talbot–Lau grating interferometry is a new innovative X-ray technology in the field of radiography and computed tomography that extends the imaging capabilities of absorption contrast (AC in medicine and material science by the introduction of differential phase contrast (DPC and dark-field contrast (DFC. This paper discusses the benefits of the additional imaging modality of DFC provided by a new desktop Talbot–Lau μXCT system (SkyScan 1294. With this system, selected medical and biological samples such as medical foam, cortical bone, molar tooth, and barley corn seed samples have been imaged and compared to reference methods such as high-resolution μXCT and optical coherence tomography (OCT regarding information gain and contrast.

  9. Determination of trace elements in biological samples treated with formic acid by inductively coupled plasma mass spectrometry using a microconcentric nebulizer

    International Nuclear Information System (INIS)

    Tormen, Luciano; Gil, Raul A.; Frescura, Vera L.A.; Dante Martinez, Luis; Curtius, Adilson J.

    2010-01-01

    A simple and fast method for the determination of As, Ba, Cd, Co, Cu, Fe, Ga, Mn, Mo, Ni, Pb, Rb, Se, Sr, Tl, U, V and Zn in biological samples by inductively coupled plasma mass spectrometry (ICP-MS), after sample solubilization with formic acid and introduction by a microconcentric nebulizer, is proposed. The sample is mixed with formic acid, kept at 90 o C for one hour and then diluted with nitric acid aqueous solution to a 50% v/v formic acid and 1% v/v nitric acid final concentrations. The final sample solution flow rate for introduction into the plasma was 30 μL min -1 . The optimized and adopted nebulizer gas flow rate was 0.7 L min -1 and RF power was 800 W. These conditions are very different than those normally used when a conventional nebulizer is employed. Rodhium was used as internal standard. External calibration against aqueous standard solutions, without formic acid, could be used for quantification, except for As, Se and Zn. However, external calibration with 50% formic acid allows the determination of all analytes with high accuracy and it is recommended. The detection limits were between 0.0005 (Tl) and 0.22 mg kg -1 (Fe) and the precision expressed by the relative standard deviations (RSD) were between 0.2% (Sr) and 3.5% (Ga). Accuracy was validated by the analysis of four certified reference biological materials of animal tissues, comparing the results by linear regressions and by the t-test at a 95% confidence level. The recommended procedure avoids plasma instability and carbon deposit on the cones.

  10. Determination of thallium at ultra-trace levels in water and biological samples using solid phase spectrophotometry.

    Science.gov (United States)

    Amin, Alaa S; El-Sharjawy, Abdel-Azeem M; Kassem, Mohammed A

    2013-06-01

    A new simple, very sensitive, selective and accurate procedure for the determination of trace amounts of thallium(III) by solid-phase spectrophotometry (SPS) has been developed. The procedure is based on fixation of Tl(III) as quinalizarin ion associate on a styrene-divinylbenzene anion-exchange resin. The absorbance of resin sorbed Tl(III) ion associate is measured directly at 636 and 830 nm. Thallium(I) was determined by difference measurements after oxidation of Tl(I) to Tl(III) with bromine. Calibration is linear over the range 0.5-12.0 μg L(-1) of Tl(III) with relative standard deviation (RSD) of 1.40% (n=10). The detection and quantification limits are 150 and 495 ng L(-1) using 0.6 g of the exchanger. The molar absorptivity and Sandell sensitivity are also calculated and found to be 1.31×10(7) L mol(-1)cm(-1) and 0.00156 ng cm(-2), respectively. The proposed procedure has been successfully applied to determine thallium in water, urine and serum samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  11. Sensitive and Rapid UHPLC-MS/MS for the Analysis of Tomato Phenolics in Human Biological Samples

    Directory of Open Access Journals (Sweden)

    Miriam Martínez-Huélamo

    2015-11-01

    Full Text Available An UHPLC-MS/MS method for the quantification of tomato phenolic metabolites in human fluids was optimized and validated, and then applied in a pilot dietary intervention study with healthy volunteers. A 5-fold gain in speed (3.5 min of total run; 7-fold increase in MS sensitivity and 2-fold greater efficiency (50% peak width reduction were observed when comparing the proposed method with the reference-quality HPLC-MS/MS system, whose assay performance has been previously documented. The UHPLC-MS/MS method led to an overall improvement in the limits of detection (LOD and quantification (LOQ for all the phenolic compounds studied. The recoveries ranged between 68% and 100% in urine and 61% and 100% in plasma. The accuracy; intra- and interday precision; and stability met with the acceptance criteria of the AOAC International norms. Due to the improvements in the analytical method; the total phenolic metabolites detected in plasma and urine in the pilot intervention study were 3 times higher than those detected by HPLC-MS/MS. Comparing with traditional methods; which require longer time of analysis; the methodology described is suitable for the analysis of phenolic compounds in a large number of plasma and urine samples in a reduced time frame.

  12. A disposable screen-printed silver strip sensor for single drop analysis of halide in biological samples.

    Science.gov (United States)

    Chiu, Mei-Hsin; Cheng, Wan-Ling; Muthuraman, Govindan; Hsu, Cheng-Teng; Chung, Hsieh-Hsun; Zen, Jyh-Myng

    2009-06-15

    A screen-printed silver strip with three-electrode configuration of Ag-working, Ag-counter and Ag/Ag(x)O reference electrodes was developed for simultaneous determination of chloride, bromide and iodide in aqueous solutions. It was fabricated simply by screen-printing silver ink onto a polypropylene (PP) base. The in-situ prepared Ag/Ag(x)O reference electrode can avoid the leaching interference in chloride detection while using a conventional Ag/AgCl reference electrode. A single drop of analyte (50 microl) is enough to determine iodide, bromide and chloride by measuring the well-separated oxidation peak currents of respective silver halides. The calibration graph was linear from 10 microM to 20 mM for iodide and bromide and 100 microM to 20 mM for chloride and the detection limit (S/N=3) was 3.05 microM, 2.95 microM and 18.83 microM for iodide, bromide and chloride, respectively. The strip is designed to be disposable and as such manual polishing is not necessary. The proposed sensor is not only simple to manufacture and easy to operate but also fast and precise with little detection volume. It is successfully applied to the determination of halide ions in real samples.

  13. Preparation of magnetite/poly(styrene-divinylbenzene) nanoparticles for selective enrichment-determination of fenitrothion in environmental and biological samples.

    Science.gov (United States)

    Eskandari, Habibollah; Naderi-Darehshori, Ali

    2012-09-19

    In the present study, a cross-linked nano-sized spherical magnetic poly(styrene-divinylbenzene) is synthesized and used as an adsorbent for enrichment-determination of fenitrothion. A miniemulsion polymerization procedure was used to prepare the adsorbent. The magnetic adsorbent was characterized by FT-IR, SEM and TEM. The prepared magnetic adsorbent nanoparticles were mixed with magnetite nanoparticles for faster and more efficient magnetic precipitation. The reduced fenitrothion was coupled with 3-methyl-2-benzothiazolinone hydrazone and then the blue colored complex was extracted. The blue derivative of fenitrothion was eluted by a 1 mL aliquot of 1-propanol prior to spectrophotometry at 571 nm. Beer's law was obeyed in the range of 2-230 ng mL(-1) of fenitrothion with relative standard deviation and recovery in the ranges of 0.9-5.1% and 97.2-100.0%, respectively. Selectivity of the method was evaluated, and the method was successfully applied to the determination of fenitrothion in various water, soil, urine and human plasma samples. Crown Copyright © 2012. Published by Elsevier B.V. All rights reserved.

  14. Using low-E resonators to reduce RF heating in biological samples for static solid-state NMR up to 900 MHz

    Science.gov (United States)

    Gor'kov, Peter L.; Chekmenev, Eduard Y.; Li, Conggang; Cotten, Myriam; Buffy, Jarrod J.; Traaseth, Nathaniel J.; Veglia, Gianluigi; Brey, William W.

    2007-03-01

    RF heating of solid-state biological samples is known to be a destabilizing factor in high-field NMR experiments that shortens the sample lifetime by continuous dehydration during the high-power cross-polarization and decoupling pulses. In this work, we describe specially designed, large volume, low-E15N- 1H solid-state NMR probes developed for 600 and 900 MHz PISEMA studies of dilute membrane proteins oriented in hydrated and dielectrically lossy lipid bilayers. The probes use an orthogonal coil design in which separate resonators pursue their own aims at the respective frequencies, resulting in a simplified and more efficient matching network. Sample heating at the 1H frequency is minimized by a loop-gap resonator which produces a homogeneous magnetic field B1 with low electric field E. Within the loop-gap resonator, a multi-turn solenoid closely matching the shape of the sample serves as an efficient observe coil. We compare power dissipation in a typical lossy bilayer sample in the new low-E probe and in a previously reported 15N- 1H probe which uses a double-tuned 4-turn solenoid. RF loss in the sample is measured in each probe by observing changes in the 1H 360° pulse lengths. For the same values of 1H B1 field, sample heating in the new probe was found to be smaller by an order of magnitude. Applications of the low-E design to the PISEMA study of membrane proteins in their native hydrated bilayer environment are demonstrated at 600 and 900 MHz.

  15. Employment of modified Fe3 O4 nanoparticles using thermo-sensitive polymer for extraction and pre-concentration of cefexime in biological samples.

    Science.gov (United States)

    Naghibi, Saman; Sahebi, Hamed

    2018-02-01

    Cefexime is a useful antibiotic that can be prescribed to treat bacterial infections. Nanoparticles have been widely marketed as a universal solution among scientists. Many studies have been performed to modify nanoparticles to make them functional as extraction and pre-concentration agents and drug carriers. Temperature-sensitive polymers belong to a group of substances that undergo a major change in their physical features in response to temperature. Recently developed polymers can be used in many different areas, including modification of nanoparticles. In order to modify this nanoparticle, grafting copolymerization of Fe 3 O 4 nanoparticles was performed using poly (N-vinylcaprolactam) and 3-allyloxy-1,2-propanediol. The optimum conditions for pre-concentration of cefexime were studied. Under these optimum conditions, extraction recovery of biological samples in the range of 71-89% was obtained. The limit of detection and precision of proposed method were 4.5 × 10 -4  μg mL -1 and analysis of cefexime, in biological samples using the proposed method, the ability of this method to extract and pre-concentrate cefexime was confirmed. Also, satisfactory results from an in vitro study on drug release in simulated intestine media were obtained. Copyright © 2017 John Wiley & Sons, Ltd.

  16. Mercapto-ordered carbohydrate-derived porous carbon electrode as a novel electrochemical sensor for simple and sensitive ultra-trace detection of omeprazole in biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Kalate Bojdi, Majid [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran 1983963113 (Iran, Islamic Republic of); Faculty of Chemistry, Kharazmi (Tarbiat Moallem) University, Tehran (Iran, Islamic Republic of); Behbahani, Mohammad [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran 1983963113 (Iran, Islamic Republic of); Mashhadizadeh, Mohammad Hosein [Faculty of Chemistry, Kharazmi (Tarbiat Moallem) University, Tehran (Iran, Islamic Republic of); Bagheri, Akbar [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran 1983963113 (Iran, Islamic Republic of); Hosseiny Davarani, Saied Saeed, E-mail: ss-hosseiny@sbu.ac.ir [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran 1983963113 (Iran, Islamic Republic of); Farahani, Ali [Department of Chemistry, Faculty of Science, Shahid Beheshti University, Tehran 1983963113 (Iran, Islamic Republic of)

    2015-03-01

    We are introducing mercapto-mesoporous carbon modified carbon paste electrode (mercapto-MP-C-CPE) as a new sensor for trace determination of omeprazole (OM) in biological samples. The synthesized modifier was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN) and N{sub 2} adsorption surface area measurement (BET). The electrochemical response characteristic of the modified-CPE toward OM was investigated by cyclic and differential pulse voltammetry (CV and DPV). The proposed sensor displayed a good electrooxidation response to the OM, its linear range is 0.25 nM to 25 μM with a detection limit of 0.04 nM under the optimized conditions. The prepared modified electrode shows several advantages such as high sensitivity, long-time stability, wide linear range, ease of preparation and regeneration of the electrode surface by simple polishing and excellent reproducibility. - Highlights: • A modified nanoporous carbon as a novel sensor • High stability and good repeatability and reproducibility by the prepared sensor • Trace determination of omeprazole • Biological and pharmaceutical samples.

  17. Differential pulse adsorptive stripping voltammetric determination of nanomolar levels of atorvastatin calcium in pharmaceutical and biological samples using a vertically aligned carbon nanotube/graphene oxide electrode.

    Science.gov (United States)

    Silva, Tiago Almeida; Zanin, Hudson; Vicentini, Fernando Campanhã; Corat, Evaldo José; Fatibello-Filho, Orlando

    2014-06-07

    A novel vertically aligned carbon nanotube/graphene oxide (VACNT-GO) electrode is proposed, and its ability to determine atorvastatin calcium (ATOR) in pharmaceutical and biological samples by differential pulse adsorptive stripping voltammetry (DPAdSV) is evaluated. VACNT films were prepared on a Ti substrate by a microwave plasma chemical vapour deposition method and then treated with oxygen plasma to produce the VACNT-GO electrode. The oxygen plasma treatment exfoliates the carbon nanotube tips exposing graphene foils and inserting oxygen functional groups, these effects improved the VACNT wettability (super-hydrophobic) which is crucial for its electrochemical application. The electrochemical behaviour of ATOR on the VACNT-GO electrode was studied by cyclic voltammetry, which showed that it underwent an irreversible oxidation process at a potential of +1.08 V in pHcond 2.0 (0.2 mol L(-1) buffer phosphate solution). By applying DPAdSV under optimized experimental conditions the analytical curve was found to be linear in the ATOR concentration range of 90 to 3.81 × 10(3) nmol L(-1) with a limit of detection of 9.4 nmol L(-1). The proposed DPAdSV method was successfully applied in the determination of ATOR in pharmaceutical and biological samples, and the results were in close agreement with those obtained by a comparative spectrophotometric method at a confidence level of 95%.

  18. Mercapto-ordered carbohydrate-derived porous carbon electrode as a novel electrochemical sensor for simple and sensitive ultra-trace detection of omeprazole in biological samples

    International Nuclear Information System (INIS)

    Kalate Bojdi, Majid; Behbahani, Mohammad; Mashhadizadeh, Mohammad Hosein; Bagheri, Akbar; Hosseiny Davarani, Saied Saeed; Farahani, Ali

    2015-01-01

    We are introducing mercapto-mesoporous carbon modified carbon paste electrode (mercapto-MP-C-CPE) as a new sensor for trace determination of omeprazole (OM) in biological samples. The synthesized modifier was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN) and N 2 adsorption surface area measurement (BET). The electrochemical response characteristic of the modified-CPE toward OM was investigated by cyclic and differential pulse voltammetry (CV and DPV). The proposed sensor displayed a good electrooxidation response to the OM, its linear range is 0.25 nM to 25 μM with a detection limit of 0.04 nM under the optimized conditions. The prepared modified electrode shows several advantages such as high sensitivity, long-time stability, wide linear range, ease of preparation and regeneration of the electrode surface by simple polishing and excellent reproducibility. - Highlights: • A modified nanoporous carbon as a novel sensor • High stability and good repeatability and reproducibility by the prepared sensor • Trace determination of omeprazole • Biological and pharmaceutical samples

  19. Simultaneous quantitative profiling of 20 isoprostanoids from omega-3 and omega-6 polyunsaturated fatty acids by LC-MS/MS in various biological samples.

    Science.gov (United States)

    Dupuy, Aude; Le Faouder, Pauline; Vigor, Claire; Oger, Camille; Galano, Jean-Marie; Dray, Cédric; Lee, Jetty Chung-Yung; Valet, Philippe; Gladine, Cécile; Durand, Thierry; Bertrand-Michel, Justine

    2016-05-19

    Isoprostanoids are a group of non-enzymatic oxygenated metabolites of polyunsaturated fatty acids. It belongs to oxylipins group, which are important lipid mediators in biological processes, such as tissue repair, blood clotting, blood vessel permeability, inflammation and immunity regulation. Recently, isoprostanoids from eicosapentaenoic, docosahexaenoic, adrenic and α-linolenic namely F3-isoprostanes, F4-neuroprostanes, F2-dihomo-isoprostanes and F1-phytoprostanes, respectively have attracted attention because of their putative contribution to health. Since isoprostanoids are derived from different substrate of PUFAs and can have similar or opposing biological consequences, a total isoprostanoids profile is essential to understand the overall effect in the testing model. However, the concentration of most isoprostanoids range from picogram to nanogram, therefore a sensitive method to quantify 20 isoprostanoids simultaneously was formulated and measured by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The lipid portion from various biological samples was extracted prior to LC-MS/MS evaluation. For all the isoprostanoids LOD and LOQ, and the method was validated on plasma samples for matrix effect, yield of extraction and reproducibility were determined. The methodology was further tested for the isoprostanoids profiles in brain and liver of LDLR(-/-) mice with and without docosahexaenoic acid (DHA) supplementation. Our analysis showed similar levels of total F2-isoprostanes and F4-neuroprostanes in the liver and brain of non-supplemented LDLR(-/-) mice. The distribution of different F2-isoprostane isomers varied between tissues but not for F4-neuroprostanes which were predominated by the 4(RS)-4-F4t-neuroprostane isomer. DHA supplementation to LDLR(-/-) mice concomitantly increased total F4-neuroprostanes levels compared to F2-isoprostanes but this effect was more pronounced in the liver than brain. Copyright © 2016 Elsevier B.V. All rights

  20. A novel, fully-automated, chemiluminescent assay for the detection of 1,25-dihydroxyvitamin D in biological samples.

    Science.gov (United States)

    Valcour, Andre; Zierold, Claudia; Podgorski, Angela L; Olson, Gregory T; Wall, John V; DeLuca, Hector F; Bonelli, Fabrizio

    2016-11-01

    1,25-Dihydroxyvitamin D (1,25-(OH) 2 D), the hormonal form of vitamin D, is difficult to measure because of its low circulating levels (pg/mL), and similarity to more abundant metabolites. Here a fully-automated chemiluminescent assay that accurately and precisely measures 1,25-(OH) 2 D is described. The novel 1,25-(OH) 2 D assay was conceived based on four pillars: (1) the VDR's ligand binding domain (LBD) as a capture molecule; (2) reaction conditions wherein 1,25-(OH) 2 D favors binding to LBD vs. the vitamin D binding protein; (3) exploitation of liganded-LBD's conformational change; (4) a monoclonal antibody specific to liganded-LBD. This specific, conformational, sandwich approach, unique for automated measurement of haptens, is superior to more cumbersome, conventional competitive formats. Accuracy of the 1,25-(OH) 2 D assay was corroborated by its alignment against LC-MS/MS with fit Deming regression equations of y=0.98x + 1.93 (r=0.92), and y=1.07x+3.77 (r=0.94) for different methods from Endocrine Sciences, Laboratory Corporation of America ® and the University of Washington, respectively. Good analytical precision was manifested by its low estimated limit of quantitation (1.57pg/mL), average intra-assay imprecision (3.5%CV; range 1.1-4.7%), and average inter-assay imprecision (4.5%CV; range 3.4-7.2%). Expected and measured recovery values were congruent (93.4% mean). The novel 1,25-(OH) 2 D method exhibited excellent correlation with well validated LC-MS/MS assays from two laboratories. Significantly, its 65min turn-around time is quicker, and sample volume smaller (75μl) than current methods. Copyright © 2015 The Authors. Published by Elsevier Ltd.. All rights reserved.

  1. Development of a novel 96-well format for liquid-liquid microextraction and its application in the HPLC analysis of biological samples.

    Science.gov (United States)

    Borijihan, Guirong; Li, Youxin; Gao, Jianguo; Bao, James J

    2014-05-01

    A novel 96-well liquid-liquid microextraction system combined with modern HPLC was developed and used for the simultaneous analysis of 96 biological samples. The system made use of hollow fibers, a 96-well plate, and a plastic base with a center hole and a side hole. One end of the hollow fiber was sealed, while the other end was attached to one of the holes positioned at the center for the plastic base. The needle was inserted into the liquid from inside or outside of the hollow fiber through the center or the side holes, respectively. The system was tested with plasma samples containing three compounds, acidic indomethacin, neutral dexamethasone, and basic propafenone. Some parameters, such as the kind and dimension of hollow fiber, pH and salt concentration of the donor phase, the selection of organic solvent for the acceptor phase, and the extraction time were investigated. Under the optimization conditions, the Log D and drug concentration of indomethacin, dexamethasone, and propafenone in plasma and urine samples were analyzed. Then, the methodology was validated. The results demonstrated that ng/mL levels could be exactly and rapidly analyzed by our system, which was equipped with an auto-injection sampler, making sample analysis more convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Determination of Iodate in Food, Environmental, and Biological Samples after Solid-Phase Extraction with Ni-Al-Zr Ternary Layered Double Hydroxide as a Nanosorbent

    Directory of Open Access Journals (Sweden)

    Hossein Abdolmohammad-Zadeh

    2012-01-01

    Full Text Available Nanostructured nickel-aluminum-zirconium ternary layered double hydroxide was successfully applied as a solid-phase extraction sorbent for the separation and pre-concentration of trace levels of iodate in food, environmental and biological samples. An indirect method was used for monitoring of the extracted iodate ions. The method is based on the reaction of the iodate with iodide in acidic solution to produce iodine, which can be spectrophotometrically monitored at 352 nm. The absorbance is directly proportional to the concentration of iodate in the sample. The effect of several parameters such as pH, sample flow rate, amount of nanosorbent, elution conditions, sample volume, and coexisting ions on the recovery was investigated. In the optimum experimental conditions, the limit of detection (3s and enrichment factor were 0.12 μg mL−1 and 20, respectively. The calibration graph using the preconcentration system was linear in the range of 0.2–2.8 μg mL−1 with a correlation coefficient of 0.998. In order to validate the presented method, a certified reference material, NIST SRM 1549, was also analyzed.

  3. A liquid chromatography-mass spectrometry method based on class characteristic fragmentation pathways to detect the class of indole-derivative synthetic cannabinoids in biological samples.

    Science.gov (United States)

    Mazzarino, Monica; de la Torre, Xavier; Botrè, Francesco

    2014-07-21

    This article describes a liquid chromatographic/tandem mass spectrometric method, based on the use of precursor ion scan as the acquisition mode, specifically developed to detect indole-derived cannabinoids (phenylacetylindoles, naphthoylindoles and benzoylindoles) in biological fluids (saliva, urine and blood). The method is designed to recognize one or more common "structural markers", corresponding to mass spectral fragments originating from the specific portion of the molecular structure that is common to the aminoalkylindole analogues and that is fundamental for their pharmacological classification. As such, the method is also suitable for detecting unknown substances, provided they contain the targeted portion of the molecular structure. The pre-treatment procedure consists in a liquid/liquid extraction step carried out at neutral pH: this is the only pretreatment in the case of analyses carried out in saliva, while it follows an enzymatic hydrolysis procedure in the case of urine samples, or a protein precipitation step in the case of blood samples. The chromatographic separation is achieved using an octadecyl reverse-phase 5 μm fused-core particle column; while the mass spectrometric detection is carried out by a triple-quadrupole instrument in positive electrospray ionization and precursor ion scan as acquisition mode, selecting, as mass spectral fragments, the indole (m/z 144), the carbonylnaphthalenyl (m/z 155) and the naphthalenyl (m/z 127) moieties. Once developed and optimized, the analytical procedure was validated in term of sensitivity (lower limits of detection in the range of 0.1-0.5 ng mL(-1)), specificity (no interference was detected at the retention times of the analytes under investigation), recovery (higher than 65% with a satisfactory repeatability: CV% lower than 10), matrix effect (lower than 30% for all the biological specimens tested), repeatability of the retention times (CV% lower than 0.1), robustness, and carry over (the positive

  4. The Multi-Template Molecularly Imprinted Polymer Based on SBA-15 for Selective Separation and Determination of Panax notoginseng Saponins Simultaneously in Biological Samples

    Directory of Open Access Journals (Sweden)

    Chenghong Sun

    2017-11-01

    Full Text Available The feasible, reliable and selective multi-template molecularly imprinted polymers (MT-MIPs based on SBA-15 (SBA-15@MT-MIPs for the selective separation and determination of the trace level of ginsenoside Rb1 (Rb1, ginsenoside Rg1 (Rg1 and notoginsenoside R1 (R1 simultaneously from biological samples were developed. The polymers were constructed by SBA-15 as support, Rb1, Rg1, R1 as multi-template, acrylamide (AM as functional monomer and ethylene glycol dimethacrylate (EGDMA as cross-linker. The new synthetic SBA-15@MT-MIPs were satisfactorily applied to solid-phase extraction (SPE coupled with high performance liquid chromatography (HPLC for the separation and determination of trace Rb1, Rg1 and R1 in plasma samples. Under the optimized conditions, the limits of detection (LODs and quantitation (LOQs of the proposed method for Rb1, Rg1 and R1 were in the range of 0.63–0.75 ng·mL−1 and 2.1–2.5 ng·mL−1, respectively. The recoveries of R1, Rb1 and Rg1 were obtained between 93.4% and 104.3% with relative standard deviations (RSDs in the range of 3.3–4.2%. All results show that the obtained SBA-15@MT-MIPs could be a promising prospect for the practical application in the selective separation and enrichment of trace Panax notoginseng saponins (PNS in the biological samples.

  5. The Design and Transformation of Biofundamentals: A Nonsurvey Introductory Evolutionary and Molecular Biology Course

    Science.gov (United States)

    Klymkowsky, Michael W.; Rentsch, Jeremy D.; Begovic, Emina; Cooper, Melanie M.

    2016-01-01

    Many introductory biology courses amount to superficial surveys of disconnected topics. Often, foundational observations and the concepts derived from them and students' ability to use these ideas appropriately are overlooked, leading to unrealistic expectations and unrecognized learning obstacles. The result can be a focus on memorization at the…

  6. Genetic predisposition to advanced biological ageing increases risk for childhood-onset recurrent major depressive disorder in a large UK sample.

    Science.gov (United States)

    Michalek, Julia E; Kepa, Agnieszka; Vincent, John; Frissa, Souci; Goodwin, Laura; Hotopf, Matthew; Hatch, Stephani L; Breen, Gerome; Powell, Timothy R

    2017-04-15

    Previous studies have revealed increased biological ageing amongst major depressive disorder (MDD) patients, as assayed by shorter leukocyte telomere lengths (TL). Stressors such as childhood maltreatment are more common amongst MDD patients, and it has been suggested that this might contribute to shorter TL present amongst patients. However, to our knowledge, no study has yet tested for reverse causality, i.e. whether a genetic predisposition to shorter TL might predispose to MDD or an earlier onset of MDD. This study used a Mendelian randomisation design to investigate if shortened TL might increase risk for recurrent MDD in a relatively large UK sample (1628 MDD cases, 1140 controls). To achieve this, we used a subset of our sample, for which TL data was available, to identify a suitable instrumental variable. We performed single nucleotide polymorphism (SNP) genotyping on rs10936599, a SNP upstream of telomerase RNA component (TERC), and rs2736100, a SNP within telomerase reverse transcriptase (hTERT), and attempted to replicate findings which identified these SNPs as predictors of TL. After which, we performed regressions to test if genetic risk for shortened TL increased risk for MDD, childhood-onset MDD or childhood/adolescent-onset MDD. T-carriers of rs10936599 demonstrated shorter TL compared to CC-carriers (p≤0.05; 3% of variance explained) and was subsequently used as our instrumental variable. We found that the T-allele of rs10936599 predicted increased risk for childhood-onset MDD relative to controls (p≤0.05), and increased risk for childhood-onset MDD relative to adult-onset MDD cases (p≤0.001), but rs10936599 did not predict adult-onset MDD risk. Limitations include a relatively small sample of early-onset cases, and the fact that age-of-onset was ascertained by retrospective recall. Genetic predisposition to advanced biological ageing, as assayed using rs10936599, predicted a small, but significant, increased risk for childhood

  7. Rapid ionic liquid-based ultrasound assisted dual magnetic microextraction to preconcentrate and separate cadmium-4-(2-thiazolylazo)-resorcinol complex from environmental and biological samples.

    Science.gov (United States)

    Khan, Sumaira; Kazi, Tasneem Gul; Soylak, Mustafa

    2014-04-05

    A rapid and innovative microextraction technique named as, ionic liquid-based ultrasound-assisted dual magnetic microextraction (IL-UA-DMME) was developed for the preconcentration and extraction of trace cadmium from environmental and biological samples, prior to analyzed by flame atomic absorption spectrometry (FAAS). The proposed method has many obvious advantages, including evading the use of organic solvents and achieved high extraction yields by the combination of dispersive liquid-liquid microextraction (DLLME) and magnetic mediated-solid phase extraction (MM-SPE). In this approach ionic liquid (IL) 1-butyl-3-methylimidazolium hexafluorophosphate [C4mim][PF6] play an important role to extract the cadmium-4-(2-thiazolylazo)-resorcinol (Cd-TAR) complex from acid digested sample solutions and ultrasonic irradiation was applied to assist emulsification. After then, dispersed small amount of Fe3O4 magnetic nanoparticles (MNPs) in sample solutions to salvaged the IL and complete phase separation was attained. Some analytical parameters that influencing the efficiency of proposed (IL-UA-DMME) method, such as pH, volume of IL, ligand concentration, ultra-sonication time, amount of Fe3O4 MNPs, sample volume and matrix effect were optimized. Limit of detection (LOD) and enrichment factor (EF) of the method under optimal experimental conditions were found to be 0.40μgL(-1) and 100, respectively. The relative standard deviation (RSD) of 50μgL(-1) Cd was 4.29%. The validity and accuracy of proposed method, was assessed to analyzed certified reference materials of fortified lake water TMDA-54.4, SPS-WW2 waste water, spinach leaves 1570a and also checked by standard addition method. The obtained values showed good agreement with the certified values and sufficiently high recovery were found in the range of 98.1-101% for Cd. The proposed method was facile, rapid and successfully applied for the determination of Cd in environmental and different biological samples

  8. Multiplex Real-Time PCR Assay Using TaqMan Probes for the Identification of Trypanosoma cruzi DTUs in Biological and Clinical Samples

    Science.gov (United States)

    Cura, Carolina I.; Duffy, Tomas; Lucero, Raúl H.; Bisio, Margarita; Péneau, Julie; Jimenez-Coello, Matilde; Calabuig, Eva; Gimenez, María J.; Valencia Ayala, Edward; Kjos, Sonia A.; Santalla, José; Mahaney, Susan M.; Cayo, Nelly M.; Nagel, Claudia; Barcán, Laura; Málaga Machaca, Edith S.; Acosta Viana, Karla Y.; Brutus, Laurent; Ocampo, Susana B.; Aznar, Christine; Cuba Cuba, Cesar A.; Gürtler, Ricardo E.; Ramsey, Janine M.; Ribeiro, Isabela; VandeBerg, John L.; Yadon, Zaida E.; Osuna, Antonio; Schijman, Alejandro G.

    2015-01-01

    Background Trypanosoma cruzi has been classified into six Discrete Typing Units (DTUs), designated as TcI–TcVI. In order to effectively use this standardized nomenclature, a reproducible genotyping strategy is imperative. Several typing schemes have been developed with variable levels of complexity, selectivity and analytical sensitivity. Most of them can be only applied to cultured stocks. In this context, we aimed to develop a multiplex Real-Time PCR method to identify the six T. cruzi DTUs using TaqMan probes (MTq-PCR). Methods/Principal Findings The MTq-PCR has been evaluated in 39 cultured stocks and 307 biological samples from vectors, reservoirs and patients from different geographical regions and transmission cycles in comparison with a multi-locus conventional PCR algorithm. The MTq-PCR was inclusive for laboratory stocks and natural isolates and sensitive for direct typing of different biological samples from vectors, reservoirs and patients with acute, congenital infection or Chagas reactivation. The first round SL-IR MTq-PCR detected 1 fg DNA/reaction tube of TcI, TcII and TcIII and 1 pg DNA/reaction tube of TcIV, TcV and TcVI reference strains. The MTq-PCR was able to characterize DTUs in 83% of triatomine and 96% of reservoir samples that had been typed by conventional PCR methods. Regarding clinical samples, 100% of those derived from acute infected patients, 62.5% from congenitally infected children and 50% from patients with clinical reactivation could be genotyped. Sensitivity for direct typing of blood samples from chronic Chagas disease patients (32.8% from asymptomatic and 22.2% from symptomatic patients) and mixed infections was lower than that of the conventional PCR algorithm. Conclusions/Significance Typing is resolved after a single or a second round of Real-Time PCR, depending on the DTU. This format reduces carryover contamination and is amenable to quantification, automation and kit production. PMID:25993316

  9. Reprint of: Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    International Nuclear Information System (INIS)

    Zarzycki, Paweł K.; Ślączka, Magdalena M.; Zarzycka, Magdalena B.; Włodarczyk, Elżbieta; Baran, Michał J.

    2012-01-01

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds’ feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5–8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  10. Reprint of: Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Zarzycki, Pawel K., E-mail: pawel_k_z@hotmail.com [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland); Slaczka, Magdalena M.; Zarzycka, Magdalena B.; Wlodarczyk, Elzbieta; Baran, Michal J. [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland)

    2012-02-24

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  11. Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    International Nuclear Information System (INIS)

    Zarzycki, Pawel K.; Slaczka, Magdalena M.; Zarzycka, Magdalena B.; Wlodarczyk, Elzbieta; Baran, Michal J.

    2011-01-01

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  12. Application of micro-thin-layer chromatography as a simple fractionation tool for fast screening of raw extracts derived from complex biological, pharmaceutical and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Zarzycki, Pawel K., E-mail: pawel_k_z@hotmail.com [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland); Slaczka, Magdalena M.; Zarzycka, Magdalena B.; Wlodarczyk, Elzbieta; Baran, Michal J. [Section of Toxicology and Bioanalytics, Department of Civil and Environmental Engineering, Koszalin University of Technology, Sniadeckich 2, 75-453 Koszalin (Poland)

    2011-03-04

    The main goal of present paper is to demonstrate the separation and detection capability of micro-TLC technique involving simple one step liquid extraction protocols of complex materials without multi-steps sample pre-purification. In the present studies target components (cyanobacteria pigments, lipids and fullerenes) were isolated from heavy loading complex matrices including spirulina dried cells, birds' feathers and fatty oils as well as soot samples derived from biomass fuel and fossils-fired home heating systems. In each case isocratic separation protocol involving less that 1 mL of one component or binary mixture mobile phases can be completed within time of 5-8 min. Sensitive detection of components of interest was performed via fluorescence or staining techniques using iodine or phosphomolybdic acid. Described methodology can be applied for fast fractionation or screening of whole range of target substances as well as chemo-taxonomic studies and fingerprinting of complex mixtures, which are present in raw biological or environmental samples.

  13. Preconcentration of trace amounts of formaldehyde from water, biological and food samples using an efficient nanosized solid phase, and its determination by a novel kinetic method

    International Nuclear Information System (INIS)

    Afkhami, A.; Bagheri, H.

    2012-01-01

    This work presents a sensitive method for the determination of formaldehyde. It is based on the use of modified alumina nanoparticles for its preconcentration, this followed by a new and simple catalytic kinetic method for its determination. Alumina nanoparticles were chemically modified by immobilization of 2,4-dinitrophenylhydrazine via sodium dodecyl sulfate as a surfactant. The formaldehyde retained on the modified adsorbent was then desorbed and determined via its catalytic effect on the oxidation of thionine by bromate ion. Factors affecting the preconcentration and determination of formaldehyde have been investigated. Formaldehyde can be detected in the range from 0. 05 to 38. 75 μg L -1 , and no serious interferences have been observed. The method has been successfully applied to the quantitation of formaldehyde in water, food, and certain biological samples. (author)

  14. A Simple Spectrophotometric Method for the Determination of Copper in Some Real, Environmental, Biological, Food and Soil Samples Using Salicylaldehyde Benzoyl Hydrazone

    Directory of Open Access Journals (Sweden)

    M. Jamaluddin Ahmed

    2012-06-01

    Full Text Available A very simple, ultra-sensitive, highly selective and non-extractive spectrophotometric method for the determination of trace amounts copper(II has been developed. Salicylaldehy debenzoyl hydrazone (SAL-BH has been proposed as a new analytical reagent for the direct non-extractive spectrophotometric determination of copper(II. SAL-BH reacts with copper in a slightly acidic (0.0001-0.005 M H2SO4 in 40% 1,4-dioxane media with copper(II to give a highly absorbent greenish yellow chelate with a molar ratio 1:1(CuII: SAL-BH The reaction is instantaneous and the maximum absorption was obtained at 404 nm and remains stable for 72 h. The average molar absorptivity and Sandell’s sensitivity were found to be 1.4×105 L mol-1 cm-1 and 5.0 ng cm-2 of copper(II, respectively. Linear calibration graphs were obtained for 0.01 – 18 mg L-1 of CuII. The detection limit and quantification limit of the reaction system were found to be 1 ng mL-1 and 10 µg L-1, respectively. A large excess of over 50 cations, anions and complexing agents (e.g., tartrate, oxalate, citrate, phosphate, thiocyanate etc. do not interfere in the determination. The method is highly selective for copper and was successfully used for the determination of copper in several standard reference materials (steels and alloys as well as in some environmental waters (portable and polluted, biological (human blood and urine, food and soil samples and solutions containing both copper(I and copper(II as well as some complex synthetic mixtures. The results of the proposed method for biological and food samples were comparable with AAS and were found to be in good agreement. The method has high precision and accuracy (s = ± 0.01 for 0.5 mg L-1.

  15. Electrochemically reduced graphene oxide-based electrochemical sensor for the sensitive determination of ferulic acid in A. sinensis and biological samples

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Linjie [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Gou, Yuqiang [Lanzhou Military Command Center for Disease Prevention and Control, Lanzhou 730000 (China); Gao, Xia; Zhang, Pei; Chen, Wenxia; Feng, Shilan [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Hu, Fangdi, E-mail: hufd@lzu.edu.cn [School of Pharmacy, Lanzhou University, Lanzhou 730000 (China); Li, Yingdong, E-mail: lydj412@163.com [Gansu College of Tradition Chinese Medicine, Lanzhou 730000 (China)

    2014-09-01

    An electrochemically reduced graphene oxide (ERGO) modified glassy carbon electrode (GCE) was used as a new voltammetric sensor for the determination of ferulic acid (FA). The morphology and microstructure of the modified electrodes were characterized by scanning electron microscopy (SEM) and Raman spectroscopy analysis, and the electrochemical effective surface areas of the modified electrodes were also calculated by chronocoulometry method. Sensing properties of the electrochemical sensor were investigated by means of cyclic voltammetry (CV) and differential pulse voltammetry (DPV). It was found that ERGO was electrodeposited on the surface of GCE by using potentiostatic method. The proposed electrode exhibited electrocatalytic activity to the redox of FA because of excellent electrochemical properties of ERGO. The transfer electron number (n), electrode reaction rate constant (k{sub s}) and electron-transfer coefficient (α) were calculated as 1.12, 1.24 s{sup −1}, and 0.40, respectively. Under the optimized conditions, the oxidation peak current was proportional to FA concentration at 8.49 × 10{sup −8} mol L{sup −1} to 3.89 × 10{sup −5} mol L{sup −1} with detection limit of 2.06 × 10{sup −8} mol L{sup −1}. This fabricated sensor also displayed acceptable reproducibility, long-term stability, and high selectivity with negligible interferences from common interfering species. The voltammetric sensor was successfully applied to detect FA in A. sinensis and biological samples with recovery values in the range of 99.91%-101.91%. - Highlights: • A novel ERGO–based electrochemical sensor of FA was successfully fabricated by using one-step electrodeposition method. • The electrode reaction was an adsorption–diffusion mixed controlled process. • The low detection limit with good selectivity and sensitivity were obtained. • This method was applied for the determination of FA in A. sinensis and biological samples.

  16. Characterization of L-cysteine capped CdTe quantum dots and application to test Cu(II) deficiency in biological samples from critically ill patients

    International Nuclear Information System (INIS)

    Sáez, Laura; Molina, Jorge; Florea, Daniela I.; Planells, Elena M.; Cabeza, M. Carmen; Quintero, Bartolomé

    2013-01-01

    Graphical abstract: -- Highlights: •We examinate stability of L-cysteine capped CdTe QD. •Factors influence QD fluorescence response are controlled. •Application in copper deficiency analysis is made. •We report comparison with other techniques. -- Abstract: The catalytic activity of copper ion gives, from the physiological point of view, a central role in many biological processes. Variations in the composition and location of cellular copper have been addressed given their physiological and pathological consequences. In this paper L-cysteine capped CdTe quantum dots is used for the fluorimetric determination of Cu(II) in biological samples from healthy individuals and patients admitted to the Intensive Care Units (ICU). An acceptable homogeneity in the CdTe QDs size has been obtained with an average value of 3 nm. No significant alterations in the spectral properties were observed for 2 months when stored in vacutainers at 6 °C and a concentration of approximately 2 μM. Data from oxidative stress markers such superoxide dismutase, total antioxidant capacity and DNA damage can be correlated with a Cu(II) deficiency for the ICU patients as measured by flame-atomic absorption spectroscopy (FAAS) and inductively coupled plasma source mass spectrometry (ICP-MS). Aqueous solutions 0.3 μM of L-cysteine capped CdTe QDs in MOPS buffer (6 mM, pH 7.4) used at 21 °C in the range 15–60 min after preparation of the sample for the measurements of fluorescence gives contents in Cu(II) for erythrocytes in good agreement with those obtained in FAAS and ICP-MS but the comparative ease of use makes the fluorimetric technique more suitable than the other two techniques for routine analysis

  17. Characterization of L-cysteine capped CdTe quantum dots and application to test Cu(II) deficiency in biological samples from critically ill patients

    Energy Technology Data Exchange (ETDEWEB)

    Sáez, Laura; Molina, Jorge; Florea, Daniela I.; Planells, Elena M. [Institute of Nutrition and Food Technology and Department of Physiology, Faculty of Pharmacy, Campus Cartuja, University of Granada, E-18071 Granada (Spain); Cabeza, M. Carmen [Department of Physical Chemistry, Faculty of Pharmacy, University of Granada, E-18071 Granada (Spain); Quintero, Bartolomé, E-mail: bqosso@ugr.es [Department of Physical Chemistry, Faculty of Pharmacy, University of Granada, E-18071 Granada (Spain)

    2013-06-27

    Graphical abstract: -- Highlights: •We examinate stability of L-cysteine capped CdTe QD. •Factors influence QD fluorescence response are controlled. •Application in copper deficiency analysis is made. •We report comparison with other techniques. -- Abstract: The catalytic activity of copper ion gives, from the physiological point of view, a central role in many biological processes. Variations in the composition and location of cellular copper have been addressed given their physiological and pathological consequences. In this paper L-cysteine capped CdTe quantum dots is used for the fluorimetric determination of Cu(II) in biological samples from healthy individuals and patients admitted to the Intensive Care Units (ICU). An acceptable homogeneity in the CdTe QDs size has been obtained with an average value of 3 nm. No significant alterations in the spectral properties were observed for 2 months when stored in vacutainers at 6 °C and a concentration of approximately 2 μM. Data from oxidative stress markers such superoxide dismutase, total antioxidant capacity and DNA damage can be correlated with a Cu(II) deficiency for the ICU patients as measured by flame-atomic absorption spectroscopy (FAAS) and inductively coupled plasma source mass spectrometry (ICP-MS). Aqueous solutions 0.3 μM of L-cysteine capped CdTe QDs in MOPS buffer (6 mM, pH 7.4) used at 21 °C in the range 15–60 min after preparation of the sample for the measurements of fluorescence gives contents in Cu(II) for erythrocytes in good agreement with those obtained in FAAS and ICP-MS but the comparative ease of use makes the fluorimetric technique more suitable than the other two techniques for routine analysis.

  18. Flow Injection Analysis Coupled with Carbon Electrodes as the Tool for Analysis of Naphthoquinones with Respect to Their Content and Functions in Biological Samples

    Directory of Open Access Journals (Sweden)

    Rene Kizek

    2006-11-01

    Full Text Available Naphthoquinones are one of the groups of secondary metabolites widespread innature, where they mostly appear as chromatic pigments. They embody broad-range ofbiological actions from phytotoxic to fungicidal. An anticancer effect of naphthoquinonesstimulates an interest in determination and characterization of single derivatives of 1,2- and1,4-quinones in biological samples. The main aim of this work was to suggest a techniquesuitable to determine lawsone, juglone and/or plumbagin in biological samples and to studyof their influence on BY-2 tobacco cells. The BY-2 tobacco cells were cultivated in thepresence of the naphthoquinones of interest (500 μg.l-1 for 24 h and then the morphologicalchanges were observed. We found out that naphthoquinones triggered the programmed celldeath at BY-2 cells, which can be confirmed by the apoptotic bodies in nucleus. After thatwe suggested and optimized different electrochemical techniques such differential pulsevoltammetry (DPV coupled with hanging mercury drop (HMDE and carbon pasteelectrode, micro flow device coupled with carbon screen printed electrodes and flowinjection analysis coupled with Coulochem III detector to determine them. The detectionlimits of naphthoquinones of interest were expressed as 3S/N and varied from units tohundreds of ng per millilitres according to methods used. Moreover, we utilized DPVcoupled with HMDE and micro flow device to determine content of juglone in leavesPersian walnut (Juglans regia. We determined that the leaves contained juglone tenths of gper 100 g of fresh weight. The results obtained show the convincing possibilities of using ofthese methods in analysis of plant secondary metabolites.

  19. Acrylamide-functionalized graphene micro-solid-phase extraction coupled to high-performance liquid chromatography for the online analysis of trace monoamine acidic metabolites in biological samples.

    Science.gov (United States)

    Yang, Xiaoting; Hu, Yufei; Li, Gongke; Zhang, Zhuomin

    2015-05-01

    Monoamine acidic metabolites in biological samples are essential biomarkers for the diagnosis of neurological disorders. In this work, acrylamide-functionalized graphene adsorbent was successfully synthesized by a chemical functionalization method and was packed in a homemade polyether ether ketone micro column as a micro-solid-phase extraction unit. This micro-solid-phase extraction unit was directly coupled to high-performance liquid chromatography to form an online system for the separation and analysis of three monoamine acidic metabolites including homovanillic acid, 5-hydroxyindole-3-acetic acid, and 3,4-dihydroxyphenylacetic acid in human urine and plasma. The online system showed high stability, permeability, and adsorption capacity toward target metabolites. The saturated extraction amount of this online system was 213.1, 107.0, and 153.4 ng for homovanillic acid, 5-hydroxyindole-3-acetic acid, and 3,4-dihydroxyphenylacetic acid, respectively. Excellent detection limits were achieved in the range of 0.08-0.25 μg/L with good linearity and reproducibility. It was interesting that three targets in urine and plasma could be actually quantified to be 0.94-3.93 μg/L in plasma and 7.15-19.38 μg/L in urine. Good recoveries were achieved as 84.8-101.4% for urine and 77.8-95.1% for plasma with the intra- and interday relative standard deviations less than 9.3 and 10.3%, respectively. This method shows great potential for online analysis of trace monoamine acidic metabolites in biological samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Processes and procedures for a worldwide biological samples distribution; product assurance and logistic activities to support the mice drawer system tissue sharing event

    Science.gov (United States)

    Benassai, Mario; Cotronei, Vittorio

    The Mice Drawer System (MDS) is a scientific payload developed by the Italian Space Agency (ASI), it hosted 6 mice on the International Space Station (ISS) and re-entered on ground on November 28, 2009 with the STS 129 at KSC. Linked to the MDS experiment, a Tissue Sharing Program (TSP), was developed in order to make available to 16 Payload Investigators (PI) (located in USA, Canada, EU -Italy, Belgium and Germany -and Japan) the biological samples coming from the mice. ALTEC SpA (a PPP owned by ASI, TAS-I and local institutions) was responsible to support the logistics aspects of the MDS samples for the first MDS mission, in the frame of Italian Space Agency (ASI) OSMA program (OSteoporosis and Muscle Atrophy). The TSP resulted in a complex scenario, as ASI, progressively, extended the original OSMA Team also to researchers from other ASI programs and from other Agencies (ESA, NASA, JAXA). The science coordination was performed by the University of Genova (UNIGE). ALTEC has managed all the logistic process with the support of a specialized freight forwarder agent during the whole shipping operation phases. ALTEC formalized all the steps from the handover of samples by the dissection Team to the packaging and shipping process in a dedicated procedure. ALTEC approached all the work in a structured way, performing: A study of the aspects connected to international shipments of biological samples. A coopera-tive work with UNIGE/ASI /PIs to identify all the needs of the various researchers and their compatibility. A complete revision and integration of shipment requirements (addresses, tem-peratures, samples, materials and so on). A complete definition of the final shipment scenario in terms of boxes, content, refrigerant and requirements. A formal approach to identification and selection of the most suited and specialized Freight Forwarder. A clear identification of all the processes from sample dissection by PI Team, sample processing, freezing, tube preparation

  1. Selective ionic liquid ferrofluid based dispersive-solid phase extraction for simultaneous preconcentration/separation of lead and cadmium in milk and biological samples.

    Science.gov (United States)

    Fasih Ramandi, Negin; Shemirani, Farzaneh

    2015-01-01

    For the first time, a selective ionic liquid ferrofluid has been used in dispersive solid phase extraction (IL-FF-D-SPE) for simultaneous preconcentration and separation of lead and cadmium in milk and biological samples combined with flame atomic absorption spectrometry. To improve the selectivity of the ionic liquid ferrofluid, the surface of TiO2 nanoparticles with a magnetic core as sorbent was modified by loading 1-(2-pyridylazo)-2-naphtol. Due to the rapid injection of an appropriate amount of ionic liquid ferrofluid into the aqueous sample by a syringe, extraction can be achieved within a few seconds. In addition, based on the attraction of the ionic liquid ferrofluid to a magnet, no centrifugation step is needed for phase separation. The experimental parameters of IL-FF-D-SPE were optimized using a Box-Behnken design (BBD) after a Plackett-Burman screening design. Under the optimum conditions, the relative standard deviations of 2.2% and 2.4% were obtained for lead and cadmium, respectively (n=7). The limit of detections were 1.21 µg L(-1) for Pb(II) and 0.21 µg L(-1) for Cd(II). The preconcentration factors were 250 for lead and 200 for cadmium and the maximum adsorption capacities of the sorbent were 11.18 and 9.34 mg g(-1) for lead and cadmium, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. β-Cyclodextrin/thermosensitive containing polymer brushes grafted onto magnetite nano-particles for extraction and determination of venlafaxine in biological and pharmaceutical samples.

    Science.gov (United States)

    Ahmad Panahi, Homayon; Alaei, Haniyeh Sadat

    2014-12-10

    In this paper, a novel nano-sorbent is fabricated by the surface grafting of poly[β-CD/allylamine-co-N-isopropylacrylamide] onto modified magnetite nano-particles by 3-mercaptopropyltrimethoxysilane. The polymer grafted magnetite nano-particles was characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, elemental analysis, scanning electron microscopy, and transmission electron microscopy. The feasibility of employing this nano-sorbent for extraction of trace venlafaxine in pharmaceutical samples and human biological fluids are investigated. The effect of various parameters such as pH, reaction temperature, and contact time was evaluated. The result revealed that the best sorption of venlafaxine by the magnetite nano-sorbent occurred at 35 °C at an optimum pH of 5. The kinetics of the venlafaxine shows accessibility of active sites in the grafted polymer onto the drug. The equilibrium data of venlafaxine by grafted magnetite nano-sorbent are well represented by the Langmuir and Freundlich isotherm models. The adsorption capacity of venlafaxine is found 142.8 mg g(-1) and indicated the homogeneous sites onto polymer grafted magnetite nano-sorbent surface. Nearly 80% of venlafaxine was released in simulated intestinal fluid, pH 7.4, in 30 h and 90% in simulated gastric fluid, pH 1.2, in 1 h. The venlafaxine loaded-polymer grafted magnetite nano-particles were successfully applied for the extraction in urine and pharmaceutical samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. A new thiourea derivative [2-(3-ethylthioureido)benzoic acid] for cloud point extraction of some trace metals in water, biological and food samples.

    Science.gov (United States)

    Mortada, W I; Kenawy, I M M; Abdel-Rhman, M H; El-Gamal, G G; Moalla, S M N

    2017-12-01

    2-(3-Ethylthioureido)benzoic acid was prepared and characterized by electronic spectrum, elemental analysis, Fourier transform infrared spectroscopy, 1 H nuclear magnetic resonance spectrum and mass spectrum. The produced ligand was applied for the preconcentrative of Fe 3+ , Co 2+ , Cu 2+ and Zn 2+ in aqueous samples by cloud point extraction methodology. Triton X-114 was used as extractant. Experimental parameters that may affect the extraction process were examined and optimized; such as pH, ligand and triton concentrations, type of diluting solvent, extraction temperature and ionic strength. The calibration curves were linear upto 500μgL -1 for Fe 3+ , Cu 2+ and Zn 2+ and upto 200μgL -1 for Co 2+ . The achieved detection limits were 1.5, 0.23, 0.71 and 0.35μgL -1 for Fe 3+ , Co 2+ , Cu 2+ and Zn 2+ respectively. The accuracy was established by analysis of certified reference materials (Seronorm whole blood L2 and ZCS ZC85006 Tomato). The proposed procedure was used for preconcentration of these metal ions in water, biological and food samples prior to their determination by flame atomic absorption spectrometry. Copyright © 2017 Elsevier GmbH. All rights reserved.

  4. Combination of flotation and flame atomic absorption spectrometry for determination, preconcentration and separation of trace amounts of metal ions in biological samples.

    Science.gov (United States)

    Ghaedi, Mehrorang; Niknam, Khodabakhsh; Nasiri kokhdan, Syamak; Soylak, Mustafa

    2013-05-01

    An efficient enrichment procedure based on the combination of flame atomic absorption spectrometry (FAAS) and flotation for determination of Cd(2+), Ag(+) and Zn(2+) ions in various biological samples using new collector is studied. The influence of pH, amount of 2-(((1H-benzo[d]imidazol-2-yl)methoxy)methyl)-1H-benzo[d]imidazole (HBIMMHBI) as collector, sample matrix, type and amount of eluting agent, type and amount of surfactant as floating agent, ionic strength and air flow rates on the extraction efficiency were evaluated and optimized. It is ascertained that under study metal ions is preconcentrated simultaneously from matrix in the presence of 0.005 M HBIMMHBI, 0.085% (w/v) of SDS form 750 mL at pH 6.5. The floated complexes metal ions eluted quantitatively with 6 mL of 1.0 M HNO3 in methanol lead to achieve preconcentration factor of 125. The detection limits for analyte ions were in the range of 1.3-2.4 ng mL(-1), with recoveries more than 95% and relative SD lower than 4%.

  5. A new cloud point extraction procedure for determination of inorganic antimony species in beverages and biological samples by flame atomic absorption spectrometry.

    Science.gov (United States)

    Altunay, Nail; Gürkan, Ramazan

    2015-05-15

    A new cloud-point extraction (CPE) for the determination of antimony species in biological and beverages samples has been established with flame atomic absorption spectrometry (FAAS). The method is based on the fact that formation of the competitive ion-pairing complex of Sb(III) and Sb(V) with Victoria Pure Blue BO (VPB(+)) at pH 10. The antimony species were individually detected by FAAS. Under the optimized conditions, the calibration range for Sb(V) is 1-250 μg L(-1) with a detection limit of 0.25 μg L(-1) and sensitive enhancement factor of 76.3 while the calibration range for Sb(III) is 10-400 μg L(-1) with a detection limit of 5.15 μg L(-1) and sensitive enhancement factor of 48.3. The precision as a relative standard deviation is in range of 0.24-2.35%. The method was successfully applied to the speciative determination of antimony species in the samples. The validation was verified by analysis of certified reference materials (CRMs). Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Differential Mobility-Mass Spectrometry Double Spike Isotope Dilution Study of Release of β-Methylaminoalanine and Proteinogenic Amino Acids during Biological Sample Hydrolysis.

    Science.gov (United States)

    Beach, Daniel G; Kerrin, Elliott S; Giddings, Sabrina D; Quilliam, Michael A; McCarron, Pearse

    2018-01-08

    The non-protein amino acid β-methylamino-L-alanine (BMAA) has been linked to neurodegenerative disease and reported throughout the environment. Proposed mechanisms of bioaccumulation, trophic transfer and chronic toxicity of BMAA rely on the hypothesis of protein misincorporation. Poorly selective methods for BMAA analysis have led to controversy. Here, a recently reported highly selective method for BMAA quantitation using hydrophilic interaction liquid chromatography-differential mobility spectrometry-tandem mass spectrometry (HILIC-DMS-MS/MS) is expanded to include proteinogenic amino acids from hydrolyzed biological samples. For BMAA quantitation, we present a double spiking isotope dilution approach using D 3 -BMAA and 13 C 15 N 2 -BMAA. These methods were applied to study release of BMAA during acid hydrolysis under a variety of conditions, revealing that the majority of BMAA can be extracted along with only a small proportion of protein. A time course hydrolysis of BMAA from mussel tissue was carried out to assess the recovery of BMAA during sample preparation. The majority of BMAA measured by typical methods was released before a significant proportion of protein was hydrolyzed. Little change was observed in protein hydrolysis beyond typical hydrolysis times but the concentration of BMAA increased linearly. These findings demonstrate protein misincorporation is not the predominant form of BMAA in cycad and shellfish.

  7. A simple solvothermal process for fabrication of a metal-organic framework with an iron oxide enclosure for the determination of organophosphorus pesticides in biological samples.

    Science.gov (United States)

    Zhang, Suling; Jiao, Zhe; Yao, Weixuan

    2014-12-05

    An active magnetic metal-organic framework (MOF) hybrid material was prepared using a novel in situ solvothermal method in the presence of magnetite (Fe3O4) particles, that holds much promise for large-scale synthesis. MIL-101(Fe), an iron terephthalate with pore structure and high resistance to water and common solvents, was functionalized as a model with superparamagnetic qualities, using Fe3O4. The electrostatic interaction between Fe3O4 and metal ions was thereby used to chemically stabilize magnetic nanoparticles, and thus MOF crystals were uniformly enclosed by Fe3O4 to form a homogeneous magnetic product identified as a Fe3O4/MIL-101 composite. This hybrid material with magnetic susceptibility but with the lowest possible loading amount of Fe3O4 was examined, and its potential application for magnetic solid-phase extraction of six organophosphorus pesticides (OPPs) from human hair and urine samples, followed by gas chromatography analysis, was assessed. The main effect parameters including solution ionic strength, desorption solvent, extraction time and desorption time were investigated in sequence. Under optimized conditions, this method showed low detection limits (0.21-2.28 ng/mL), wide linearity, and good precision (1.8-8.7% for intra-day, 2.9-9.4% for inter-day). The matrix interference produced by hair or urine could be effectively eliminated using this method, and satisfactory recoveries of the spiked samples were 76.8-94.5% and 74.9-92.1%, respectively, indicating that the Fe3O4/MIL-101 sorbents are feasible for the analysis of trace analytes from biological samples. Copyright © 2014. Published by Elsevier B.V.

  8. Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods

    Science.gov (United States)

    Farahmand, Farnaz; Ghasemzadeh, Bahar; Naseri, Abdolhossein

    2018-01-01

    An air assisted liquid-liquid microextraction by applying the solidification of a floating organic droplet method (AALLME-SFOD) coupled with a multivariate calibration method, namely partial least squares (PLS), was introduced for the fast and easy determination of Atenolol (ATE), Propanolol (PRO) and Carvedilol (CAR) in biological samples via a spectrophotometric approach. The analytes would be extracted from neutral aqueous solution into 1-dodecanol as an organic solvent, using AALLME. In this approach a low-density solvent with a melting point close to room temperature was applied as the extraction solvent. The emulsion was immediately formed by repeatedly pulling in and pushing out the aqueous sample solution and extraction solvent mixture via a 10-mL glass syringe for ten times. After centrifugation, the extractant droplet could be simply collected from the aqueous samples by solidifying the emulsion at a lower than the melting point temperature. In the next step, analytes were back extracted simultaneously into the acidic aqueous solution. Derringer and Suich multi-response optimization were utilized for simultaneous optimizing the parameters of three analytes. This method incorporates the benefits of AALLME and dispersive liquid-liquid microextraction considering the solidification of floating organic droplets (DLLME-SFOD). Calibration graphs under optimized conditions were linear in the range of 0.30-6.00, 0.32-2.00 and 0.30-1.40 μg mL- 1 for ATE, CAR and PRO, respectively. Other analytical parameters were obtained as follows: enrichment factors (EFs) were found to be 11.24, 16.55 and 14.90, and limits of detection (LODs) were determined to be 0.09, 0.10 and 0.08 μg mL- 1 for ATE, CAR and PRO, respectively. The proposed method will require neither a highly toxic chlorinated solvent for extraction nor an organic dispersive solvent in the application process; hence, it is more environmentally friendly.

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

    Science.gov (United States)

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

    2012-01-15

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

  10. Effect of sample preparation techniques on the concentrations and distributions of elements in biological tissues using µSRXRF: a comparative study

    International Nuclear Information System (INIS)

    Al-Ebraheem, A; Dao, E; Desouza, E; McNeill, F E; Farquharson, M J; Li, C; Wainman, B C

    2015-01-01

    Routine tissue sample preparation using chemical fixatives is known to preserve the morphology of the tissue being studied. A competitive method, cryofixation followed by freeze drying, involv