Sample records for internal standard separation

  1. Measurements of Aircraft Wake Vortex Separation at High Arrival Rates and a Proposed New Wake Vortex Separation Philosophy

    NASA Technical Reports Server (NTRS)

    Rutishauser, David; Donohue, George L.; Haynie, Rudolph C.

    2003-01-01

    This paper presents data and a proposed new aircraft wake vortex separation standard that argues for a fundamental re-thinking of international practice. The current static standard, under certain atmospheric conditions, presents an unnecessary restriction on system capacity. A new approach, that decreases aircraft separation when atmospheric conditions dictate, is proposed based upon the availability of new instrumentation and a better understanding of wake physics.

  2. Assessment of Telomere Length, Phenotype, and DNA Content

    PubMed Central

    Kelesidis, Theodoros; Schmid, Ingrid

    2017-01-01

    Telomere sequences at the end of chromosomes control somatic cell division; therefore, telomere length in a given cell population provides information about its replication potential. This unit describes a method for flow cytometric measurement of telomere length in subpopulations using fluorescence in situ hybridization of fluorescently-labeled probes (Flow-FISH) without prior cell separation. After cells are stained for surface immunofluorescence, antigen-antibody complexes are covalently cross-linked onto cell membranes before FISH with a telomere-specific probe. Cells with long telomeres are included as internal standards. Addition of a DNA dye permits exclusion of proliferating cells during data analysis. DNA ploidy measurements of cells of interest and internal standard are performed on separate aliquots in parallel to Flow-FISH. Telomere fluorescence of G0/1 cells of subpopulations and internal standards obtained from Flow-FISH are normalized for DNA ploidy, and telomere length in subsets of interest is expressed as a fraction of the internal standard telomere length. PMID:28055113

  3. Assessment of Telomere Length, Phenotype, and DNA Content.

    PubMed

    Kelesidis, Theodoros; Schmid, Ingrid

    2017-01-05

    Telomere sequences at the end of chromosomes control somatic cell division; therefore, telomere length in a given cell population provides information about its replication potential. This unit describes a method for flow cytometric measurement of telomere length in subpopulations using fluorescence in situ hybridization of fluorescently-labeled probes (Flow-FISH) without prior cell separation. After cells are stained for surface immunofluorescence, antigen-antibody complexes are covalently cross-linked onto cell membranes before FISH with a telomere-specific probe. Cells with long telomeres are included as internal standards. Addition of a DNA dye permits exclusion of proliferating cells during data analysis. DNA ploidy measurements of cells of interest and internal standard are performed on separate aliquots in parallel to Flow-FISH. Telomere fluorescence of G 0/1 cells of subpopulations and internal standards obtained from Flow-FISH are normalized for DNA ploidy, and telomere length in subsets of interest is expressed as a fraction of the internal standard telomere length. © 2017 by John Wiley & Sons, Inc. Copyright © 2017 John Wiley & Sons, Inc.

  4. International Accounting and the Accounting Educator.

    ERIC Educational Resources Information Center

    Laribee, Stephen F.

    The American Assembly of Collegiate Schools of Business (AACSB) has been instrumental in internationalizing the accounting curriculum by means of accreditation requirements and standards. Colleges and universities have met the AACSB requirements either by providing separate international accounting courses or by integrating international topics…

  5. 7 CFR 51.1140 - General.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    .... paradisi and C. grandis). Separate U.S. standards apply to tangerines. The standards for internal quality... 7 Agriculture 2 2010-01-01 2010-01-01 false General. 51.1140 Section 51.1140 Agriculture Regulations of the Department of Agriculture AGRICULTURAL MARKETING SERVICE (Standards, Inspections, Marketing...

  6. Introducing a true internal standard for the Comet assay to minimize intra- and inter-experiment variability in measures of DNA damage and repair

    PubMed Central

    Zainol, Murizal; Stoute, Julia; Almeida, Gabriela M.; Rapp, Alexander; Bowman, Karen J.; Jones, George D. D.

    2009-01-01

    The Comet assay (CA) is a sensitive/simple measure of genotoxicity. However, many features of CA contribute variability. To minimize these, we have introduced internal standard materials consisting of ‘reference’ cells which have their DNA substituted with BrdU. Using a fluorescent anti-BrdU antibody, plus an additional barrier filter, comets derived from these cells could be readily distinguished from the ‘test’-cell comets, present in the same gel. In experiments to evaluate the reference cell comets as external and internal standards, the reference and test cells were present in separate gels on the same slide or mixed together in the same gel, respectively, before their co-exposure to X-irradiation. Using the reference cell comets as internal standards led to substantial reductions in the coefficient of variation (CoV) for intra- and inter-experimental measures of comet formation and DNA damage repair; only minor reductions in CoV were noted when the reference and test cell comets were in separate gels. These studies indicate that differences between individual gels appreciably contribute to CA variation. Further studies using the reference cells as internal standards allowed greater significance to be obtained between groups of replicate samples. Ultimately, we anticipate that development will deliver robust quality assurance materials for CA. PMID:19828597

  7. 25 CFR 542.42 - What are the minimum internal control standards for internal audit for Tier C gaming operations?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... maintained whose primary function is performing internal audit work and that is independent with respect to... accountability shall be reconciled to the general ledger; (ix) Information technology functions, including review... internal audit function, the accountant shall perform separate observations of the table games/gaming...

  8. 25 CFR 542.42 - What are the minimum internal control standards for internal audit for Tier C gaming operations?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... maintained whose primary function is performing internal audit work and that is independent with respect to... accountability shall be reconciled to the general ledger; (ix) Information technology functions, including review... internal audit function, the accountant shall perform separate observations of the table games/gaming...

  9. 25 CFR 542.42 - What are the minimum internal control standards for internal audit for Tier C gaming operations?

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... maintained whose primary function is performing internal audit work and that is independent with respect to... accountability shall be reconciled to the general ledger; (ix) Information technology functions, including review... internal audit function, the accountant shall perform separate observations of the table games/gaming...

  10. 25 CFR 542.42 - What are the minimum internal control standards for internal audit for Tier C gaming operations?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... maintained whose primary function is performing internal audit work and that is independent with respect to... accountability shall be reconciled to the general ledger; (ix) Information technology functions, including review... internal audit function, the accountant shall perform separate observations of the table games/gaming...

  11. Standard addition with internal standardisation as an alternative to using stable isotope labelled internal standards to correct for matrix effects-Comparison and validation using liquid chromatography-​tandem mass spectrometric assay of vitamin D.

    PubMed

    Hewavitharana, Amitha K; Abu Kassim, Nur Sofiah; Shaw, Paul Nicholas

    2018-06-08

    With mass spectrometric detection in liquid chromatography, co-eluting impurities affect the analyte response due to ion suppression/enhancement. Internal standard calibration method, using co-eluting stable isotope labelled analogue of each analyte as the internal standard, is the most appropriate technique available to correct for these matrix effects. However, this technique is not without drawbacks, proved to be expensive because separate internal standard for each analyte is required, and the labelled compounds are expensive or require synthesising. Traditionally, standard addition method has been used to overcome the matrix effects in atomic spectroscopy and was a well-established method. This paper proposes the same for mass spectrometric detection, and demonstrates that the results are comparable to those with the internal standard method using labelled analogues, for vitamin D assay. As conventional standard addition procedure does not address procedural errors, we propose the inclusion of an additional internal standard (not co-eluting). Recoveries determined on human serum samples show that the proposed method of standard addition yields more accurate results than the internal standardisation using stable isotope labelled analogues. The precision of the proposed method of standard addition is superior to the conventional standard addition method. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Separation of plant hormones from biofertilizer by capillary electrophoresis using a capillary coated dynamically with polycationic polymers.

    PubMed

    Jiang, Ting-Fu; Lv, Zhi-Hua; Wang, Yuan-Hong; Yue, Mei-E

    2006-06-01

    A new, simple and rapid capillary electrophoresis (CE) method, using hexadimethrine bromide (HDB) as electroosmotic flow (EOF) modifier, was developed for the identification and quantitative determination of four plant hormones, including gibberellin A3 (GA3), indole-3-acetic acid (IAA), alpha-naphthaleneacetic acid (NAA) and 4-chlorophenoxyacetic acid (4-CA). The optimum separation was achieved with 20 mM borate buffer at pH 10.00 containing 0.005% (w/v) of HDB. The applied voltage was -25 kV and the capillary temperature was kept constant at 25 degrees C. Salicylic acid was used as internal standard for quantification. The calibration dependencies exhibited good linearity within the ratios of the concentrations of standard samples and internal standard and the ratios of the peak areas of samples and internal standard. The correlation coefficients were from 0.9952 to 0.9997. The relative standard deviations of migration times and peak areas were < 1.93 and 6.84%, respectively. The effects of buffer pH, the concentration of HDB and the voltage on the resolution were studied systematically. By this method, the contents of plant hormone in biofertilizer were successfully determined within 7 min, with satisfactory repeatability and recovery.

  13. Fluorescein thiocarbamyl amino acids as internal standards for migration time correction in capillary sieving electrophoresis

    PubMed Central

    Pugsley, Haley R.; Swearingen, Kristian E.; Dovichi, Norman J.

    2009-01-01

    A number of algorithms have been developed to correct for migration time drift in capillary electrophoresis. Those algorithms require identification of common components in each run. However, not all components may be present or resolved in separations of complex samples, which can confound attempts for alignment. This paper reports the use of fluorescein thiocarbamyl derivatives of amino acids as internal standards for alignment of 3-(2-furoyl)quinoline-2-carboxaldehyde (FQ)-labeled proteins in capillary sieving electrophoresis. The fluorescein thiocarbamyl derivative of aspartic acid migrates before FQ-labeled proteins and the fluorescein thiocarbamyl derivative of arginine migrates after the FQ-labeled proteins. These compounds were used as internal standards to correct for variations in migration time over a two-week period in the separation of a cellular homogenate. The experimental conditions were deliberately manipulated by varying electric field and sample preparation conditions. Three components of the homogenate were used to evaluate the alignment efficiency. Before alignment, the average relative standard deviation in migration time for these components was 13.3%. After alignment, the average relative standard deviation in migration time for these components was reduced to 0.5%. PMID:19249052

  14. Improving the efficiency of quantitative (1)H NMR: an innovative external standard-internal reference approach.

    PubMed

    Huang, Yande; Su, Bao-Ning; Ye, Qingmei; Palaniswamy, Venkatapuram A; Bolgar, Mark S; Raglione, Thomas V

    2014-01-01

    The classical internal standard quantitative NMR (qNMR) method determines the purity of an analyte by the determination of a solution containing the analyte and a standard. Therefore, the standard must meet the requirements of chemical compatibility and lack of resonance interference with the analyte as well as a known purity. The identification of such a standard can be time consuming and must be repeated for each analyte. In contrast, the external standard qNMR method utilizes a standard with a known purity to calibrate the NMR instrument. The external standard and the analyte are measured separately, thereby eliminating the matter of chemical compatibility and resonance interference between the standard and the analyte. However, the instrumental factors, including the quality of NMR tubes, must be kept the same. Any deviations will compromise the accuracy of the results. An innovative qNMR method reported herein utilizes an internal reference substance along with an external standard to assume the role of the standard used in the traditional internal standard qNMR method. In this new method, the internal reference substance must only be chemically compatible and be free of resonance-interference with the analyte or external standard whereas the external standard must only be of a known purity. The exact purity or concentration of the internal reference substance is not required as long as the same quantity is added to the external standard and the analyte. The new method reduces the burden of searching for an appropriate standard for each analyte significantly. Therefore the efficiency of the qNMR purity assay increases while the precision of the internal standard method is retained. Copyright © 2013 Elsevier B.V. All rights reserved.

  15. Quantitative separation of tetralin hydroperoxide from its decomposition products by high performance liquid chromatography

    NASA Technical Reports Server (NTRS)

    Worstell, J. H.; Daniel, S. R.

    1981-01-01

    A method for the separation and analysis of tetralin hydroperoxide and its decomposition products by high pressure liquid chromatography has been developed. Elution with a single, mixed solvent from a micron-Porasil column was employed. Constant response factors (internal standard method) over large concentration ranges and reproducible retention parameters are reported.

  16. International Trade. U.S. Metric Study Interim Report.

    ERIC Educational Resources Information Center

    Gordon, Gerald F.

    In order to evaluate the potential effects of U.S. conversion to SI (Systems International) units on U.S. foreign trade, 188 export product classes and 155 import product classes were selected from 1,166 Standard Industrial Classification (SIC) product classes and questionnaires were mailed to a total of 510 firms, utilizing separate forms for…

  17. Implementing Speed and Separation Monitoring in Collaborative Robot Workcells.

    PubMed

    Marvel, Jeremy A; Norcross, Rick

    2017-04-01

    We provide an overview and guidance for the Speed and Separation Monitoring methodology as presented in the International Organization of Standardization's technical specification 15066 on collaborative robot safety. Such functionality is provided by external, intelligent observer systems integrated into a robotic workcell. The SSM minimum protective distance function equation is discussed in detail, with consideration for the input values, implementation specifications, and performance expectations. We provide analytical analyses and test results of the current equation, discuss considerations for implementing SSM in human-occupied environments, and provide directions for technological advancements toward standardization.

  18. Implementing Speed and Separation Monitoring in Collaborative Robot Workcells

    PubMed Central

    Marvel, Jeremy A.; Norcross, Rick

    2016-01-01

    We provide an overview and guidance for the Speed and Separation Monitoring methodology as presented in the International Organization of Standardization's technical specification 15066 on collaborative robot safety. Such functionality is provided by external, intelligent observer systems integrated into a robotic workcell. The SSM minimum protective distance function equation is discussed in detail, with consideration for the input values, implementation specifications, and performance expectations. We provide analytical analyses and test results of the current equation, discuss considerations for implementing SSM in human-occupied environments, and provide directions for technological advancements toward standardization. PMID:27885312

  19. Enantioselective separation of racemic juvenile hormone III by normal-phase high-performance liquid chromatography and preparation of [(2)H(3)]juvenile hormone III as an internal standard for liquid chromatography-mass spectrometry quantification.

    PubMed

    Ichikawa, Akio; Ono, Hiroshi; Furuta, Kenjiro; Shiotsuki, Takahiro; Shinoda, Tetsuro

    2007-08-17

    Juvenile hormone III (JH III) racemate was prepared from methyl (2E,6E)-farnesoate via epoxidation with 3-chloroperbenzoic acid (mCPBA). Enantioselective separation of JH III was conducted using normal-phase high-performance liquid chromatography (HPLC) on a chiral stationary phase. [(2)H(3)]Methyl (2E,6E)-farnesoate was also prepared from (2E,6E)-farnesoic acid and [(2)H(4)]methanol (methanol-d(4)) using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) and 4-dimethylaminopyridine (DMAP); the conjugated double bond underwent isomerization to some degree. Epoxidation of [(2)H(3)]methyl (2E,6E)-farnesoate with mCPBA gave a novel deuterium-substituted internal standard [(2)H(3)]JH III (JH III-d(3)). The standard curve was produced by linear regression using the peak area ratios of JH III and JH III-d(3) in liquid chromatography-mass spectrometry (LC-MS).

  20. 33 CFR 155.380 - Oily water separating equipment and bilge alarm approval standards.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) POLLUTION OIL OR HAZARDOUS MATERIAL POLLUTION... § 155.380(b): A copy of Annex I to the International Convention for the Prevention of Pollution from...

  1. Determination of Labeled Fatty Acids Content in Milk Products, Infant Formula, and Adult/Pediatric Nutritional Formula by Capillary Gas Chromatography: Collaborative Study, Final Action 2012.13.

    PubMed

    Golay, Pierre-Alain; Moulin, Julie

    2016-01-01

    A collaborative study was conducted on AOAC First Action Method 2012.13 "Determination of Labeled Fatty Acids Content in Milk Products and Infant Formula by Capillary Gas Chromatography," which is based on an initial International Organization for Standardization (ISO)-International Dairy Federation (IDF) New Work Item that has been moved forward to ISO 16958:2015|IDF 231:2015 in November 2015. It was decided to merge the two activities after the agreement signed between ISO and AOAC in June 2012 to develop common standards and to avoid duplicate work. The collaborative study was performed after having provided highly satisfactory single-laboratory validation results [Golay, P.A., & Dong, Y. (2015) J. AOAC Int. 98, 1679-1696] that exceeded the performance criteria defined in AOAC Standard Method Performance Requirement (SMPR(®)) 2012.011 (September 29, 2012) on 12 products selected by the AOAC Stakeholder Panel on Infant Formula (SPIFAN). After a qualification period of 1 month, 18 laboratories participated in the fatty acids analysis of 12 different samples in duplicate. Six samples were selected to meet AOAC SPIFAN requirements (i.e., infant formula and adult nutritionals in powder and liquid formats), and the other Six samples were selected to meet ISO-IDF requirements (i.e., dairy products such as milk powder, liquid milk, cream, butter, infant formula with milk, and cheese). The fatty acids were analyzed directly in all samples without preliminary fat extraction, except in one sample (cheese). Powdered samples were analyzed after dissolution (i.e., reconstitution) in water, whereas liquid samples (or extracted fat) were analyzed directly. After addition of the internal standards solution [C11:0 fatty acid methyl ester (FAME) and C13:0 triacylglycerols (TAG)] to the samples, fatty acids attached to lipids were transformed into FAMEs by direct transesterification using methanolic sodium methoxide. FAMEs were separated using highly polar capillary GLC and were identified by comparison with the retention times of pure analytical standards. Quantification of fatty acids was done relative to C11:0 FAME as internal standard and to instrument response factors (determined separately using calibration standards mixture). The performance of the method (i.e., transesterification) was monitored in all samples using the second internal standard, C13:0 TAG. RSDR values were summarized separately for labeled fatty acids in SPIFAN materials and ISO-IDF materials due to different expression of results. This method was applied to representative dairy, infant formula, and adult/pediatric nutritional products and demonstrated global acceptable reproducibility precision for all fatty acids analyzed (i.e., 46 individuals and/or groups) for these categories of products.

  2. Frontally eluted components procedure with thin layer chromatography as a mode of sample preparation for high performance liquid chromatography quantitation of acetaminophen in biological matrix.

    PubMed

    Klimek-Turek, A; Sikora, M; Rybicki, M; Dzido, T H

    2016-03-04

    A new concept of using thin-layer chromatography to sample preparation for the quantitative determination of solute/s followed by instrumental techniques is presented Thin-layer chromatography (TLC) is used to completely separate acetaminophen and its internal standard from other components (matrix) and to form a single spot/zone containing them at the solvent front position (after the final stage of the thin-layer chromatogram development). The location of the analytes and internal standard in the solvent front zone allows their easy extraction followed by quantitation by HPLC. The exctraction procedure of the solute/s and internal standard can proceed from whole solute frontal zone or its part without lowering in accuracy of quantitative analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

  3. Hydrophilic interaction liquid chromatography of anthranilic acid-labelled oligosaccharides with a 4-aminobenzoic acid ethyl ester-labelled dextran hydrolysate internal standard.

    PubMed

    Neville, David C A; Alonzi, Dominic S; Butters, Terry D

    2012-04-13

    Hydrophilic interaction liquid chromatography (HILIC) of fluorescently labelled oligosaccharides is used in many laboratories to analyse complex oligosaccharide mixtures. Separations are routinely performed using a TSK gel-Amide 80 HPLC column, and retention times of different oligosaccharide species are converted to glucose unit (GU) values that are determined with reference to an external standard. However, if retention times were to be compared with an internal standard, consistent and more accurate GU values would be obtained. We present a method to perform internal standard-calibrated HILIC of fluorescently labelled oligosaccharides. The method relies on co-injection of 4-aminobenzoic acid ethyl ester (4-ABEE)-labelled internal standard and detection by UV absorption, with 2-AA (2-aminobenzoic acid)-labelled oligosaccharides. 4-ABEE is a UV chromophore and a fluorophore, but there is no overlap of the fluorescent spectrum of 4-ABEE with the commonly used fluorescent reagents. The dual nature of 4-ABEE allows for accurate calculation of the delay between UV and fluorescent signals when determining the GU values of individual oligosaccharides. The GU values obtained are inherently more accurate as slight differences in gradients that can influence retention are negated by use of an internal standard. Therefore, this paper provides the first method for determination of HPLC-derived GU values of fluorescently labelled oligosaccharides using an internal calibrant. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Optimizing total reflection X-ray fluorescence for direct trace element quantification in proteins I: Influence of sample homogeneity and reflector type

    NASA Astrophysics Data System (ADS)

    Wellenreuther, G.; Fittschen, U. E. A.; Achard, M. E. S.; Faust, A.; Kreplin, X.; Meyer-Klaucke, W.

    2008-12-01

    Total reflection X-ray fluorescence (TXRF) is a very promising method for the direct, quick and reliable multi-elemental quantification of trace elements in protein samples. With the introduction of an internal standard consisting of two reference elements, scandium and gallium, a wide range of proteins can be analyzed, regardless of their salt content, buffer composition, additives and amino acid composition. This strategy also enables quantification of matrix effects. Two potential issues associated with drying have been considered in this study: (1) Formation of heterogeneous residues of varying thickness and/or density; and (2) separation of the internal standard and protein during drying (which has to be prevented to allow accurate quantification). These issues were investigated by microbeam X-ray fluorescence (μXRF) with special emphasis on (I) the influence of sample support and (II) the protein / buffer system used. In the first part, a model protein was studied on well established sample supports used in TXRF, PIXE and XRF (Mylar, siliconized quartz, Plexiglas and silicon). In the second part we imaged proteins of different molecular weight, oligomerization state, bound metals and solubility. A partial separation of protein and internal standard was only observed with untreated silicon, suggesting it may not be an adequate support material. Siliconized quartz proved to be the least prone to heterogeneous drying of the sample and yielded the most reliable results.

  5. International reference reagents: antihuman globulin. An ISBT/ICSH joint working party report. International Society of Blood Transfusion. International Committee for Standardization in Haematology.

    PubMed

    Case, J; Ford, D S; Chung, A; Collins, R; Kochman, S; Mazda, T; Overbeeke, M; Perera, R; Sakuldamrongpanich, T; Scott, M; Voak, D; Zupańska, B

    1999-01-01

    An international working party has conducted a study designed to select a suitable reference reagent for antihuman globulin, to replace those first made available in 1987. The chosen preparation contains levels of anti-IgG and anti-C3 (anti-C3c and anti-C3d) potency that are considered suitable to serve for reference when evaluating either polyspecific antihuman globulin reagents or those containing their separate monospecific components. The reference material is available in 2-ml freeze-dried aliquots from seven assigned distribution centres.

  6. International Round-Robin Testing of Bulk Thermoelectrics

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

    Wang, Hsin; Porter, Wallace D; Bottner, Harold

    2011-11-01

    Two international round-robin studies were conducted on transport properties measurements of bulk thermoelectric materials. The study discovered current measurement problems. In order to get ZT of a material four separate transport measurements must be taken. The round-robin study showed that among the four properties Seebeck coefficient is the one can be measured consistently. Electrical resistivity has +4-9% scatter. Thermal diffusivity has similar +5-10% scatter. The reliability of the above three properties can be improved by standardizing test procedures and enforcing system calibrations. The worst problem was found in specific heat measurements using DSC. The probability of making measurement error ismore » great due to the fact three separate runs must be taken to determine Cp and the baseline shift is always an issue for commercial DSC. It is suggest the Dulong Petit limit be always used as a guide line for Cp. Procedures have been developed to eliminate operator and system errors. The IEA-AMT annex is developing standard procedures for transport properties testing.« less

  7. Accreditation - ISO/IEC 17025

    NASA Astrophysics Data System (ADS)

    Kaus, Rüdiger

    This chapter gives the background on the accreditation of testing and calibration laboratories according to ISO/IEC 17025 and sets out the requirements of this international standard. ISO 15189 describes similar requirements especially tailored for medical laboratories. Because of these similarities ISO 15189 is not separately mentioned throughout this lecture.

  8. Collaborative study for the calibration of a replacement International Standard for Tetanus Toxoid Adsorbed.

    PubMed

    Tierney, Rob; Stickings, Paul; Hockley, Jason; Rigsby, Peter; Iwaki, Masaaki; Sesardic, Dorothea

    2011-11-01

    We present the results of a collaborative study for the establishment of a replacement International Standard (IS) for Tetanus Toxoid Adsorbed. Two candidate preparations were included in the study, one of which was established as the 4th IS for Tetanus Toxoid Adsorbed at the WHO Expert Committee on Biological Standardization meeting in October 2010. This preparation was found to have a unitage of 490 IU/ampoule, based on calibration in guinea pig challenge assays. Results from mouse challenge assays suggest that the relative performance of two candidate preparations may differ significantly between guinea pigs and mice. The authors note that the number of laboratories that performed guinea pig challenge assays, which are used to calibrate and assign IU, is much lower than in previous collaborative studies and this may have implications for calibration of replacement standards in the future. The issue of assigning separate units to the IS for guinea pig and mouse assays is discussed. The study also assessed performance of the replacement standard in serological assays which are used as alternative procedures to challenge assays for tetanus potency testing. Results suggest that the replacement standard is suitable for use as the reference vaccine in serological assays. Copyright © 2011 The International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

  9. Cobalt complexes as internal standards for capillary zone electrophoresis-mass spectrometry studies in biological inorganic chemistry.

    PubMed

    Holtkamp, Hannah U; Morrow, Stuart J; Kubanik, Mario; Hartinger, Christian G

    2017-07-01

    Run-by-run variations are very common in capillary electrophoretic (CE) separations and cause imprecision in both the migration times and the peak areas. This makes peak and kinetic trend identification difficult and error prone. With the aim to identify suitable standards for CE separations which are compatible with the common detectors UV, ESI-MS, and ICP-MS, the Co III complexes [Co(en) 3 ]Cl 3 , [Co(acac) 3 ] and K[Co(EDTA)] were evaluated as internal standards in the reaction of the anticancer drug cisplatin and guanosine 5'-monophosphate as an example of a classical biological inorganic chemistry experiment. These Co III chelate complexes were considered for their stability, accessibility, and the low detection limit for Co in ICP-MS. Furthermore, the Co III complexes are positively and negatively charged as well as neutral, allowing the detection in different areas of the electropherograms. The background electrolytes were chosen to cover a wide pH range. The compatibility to the separation conditions was dependent on the ligands attached to the Co III centers, with only the acetylacetonato (acac) complex being applicable in the pH range 2.8-9.0. Furthermore, because of being charge neutral, this compound could be used as an electroosmotic flow (EOF) marker. In general, employing Co complexes resulted in improved data sets, particularly with regard to the migration times and peak areas, which resulted, for example, in higher linear ranges for the quantification of cisplatin.

  10. Quantitative determination of galantamine in human plasma by sensitive liquid chromatography-tandem mass spectrometry using loratadine as an internal standard.

    PubMed

    Nirogi, Ramakrishna V S; Kandikere, Vishwottam N; Mudigonda, Koteshwara; Maurya, Santosh

    2007-02-01

    A simple, rapid, sensitive, and selective liquid chromatography-tandem mass spectrometry method is developed and validated for the quantitation of galantamine, an acetylcholinesterase inhibitor in human plasma, using a commercially available compound, loratadine, as the internal standard. Following liquid-liquid extraction, the analytes are separated using an isocratic mobile phase on a reverse-phase C18 column and analyzed by mass spectrometry in the multiple reaction monitoring mode using the respective (M+H)+ ions, m/z 288 to 213 for galantamine and m/z 383 and 337 for the internal standard. The assay exhibit a linear dynamic range of 0.5-100 ng/mL for galantamine in human plasma. The lower limit of quantitation is 0.5 ng/mL, with a relative standard deviation of less than 8%. Acceptable precision and accuracy are obtained for concentrations over the standard curve range. A run time of 2.5 min for each sample makes it possible to analyze more than 400 human plasma samples per day. The validated method is successfully used to analyze human plasma samples for application in pharmacokinetic, bioavailability, or bioequivalence studies.

  11. High-performance liquid chromatographic determination of 4,4'-dihydroxybenzophenone-2,4-dinitrophenylhydrazone in plasma.

    PubMed

    Rodgers, A H; Subramanian, S; Morgan, L R

    1995-08-18

    An analytical method has been developed for the determination of 4,4'-dihydroxybenzophenone-2,4-dinitrophenylhydrazone (I, trade name A-007) in plasma. Plasma samples are primed with the internal standard, 2,2'-dihydroxybenzophenone-2,4-dinitrophenylhydrazone (II), deproteinized with acetonitrile, centrifuged and filtered prior to assay. The components are then separated on a reversed-phase column with retention times of 4.4 and 6.0 min for I and II, respectively. Ultraviolet detection at 365 nm was employed and little interference with the analyte or the internal standard was noted from other plasma components. This method has been applied to the plasma of rats and monkeys doses for pharmacokinetic and toxicity studies.

  12. Analysis of benzo(a)pyrene in airborne particulates by gas chromatography

    NASA Technical Reports Server (NTRS)

    Luedecke, E.

    1976-01-01

    A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.

  13. Building a Science, Technology, Engineering, and Math Education Agenda: An Update of State Actions

    ERIC Educational Resources Information Center

    Thomasian, John

    2011-01-01

    STEM--science, technology, engineering, and mathematics--is critical to and supportive of many education reforms being undertaken today, from adoption of common internationally benchmarked standards to better teacher preparation to enhanced coordination across the entire K-20 education system. In fact, STEM is not a separate reform movement at…

  14. Optimization of the high-performance liquid chromatographic separation of a complex mixture containing urinary steroids, boldenone and bolasterone: application to urine samples.

    PubMed

    Gonzalo-Lumbreras, R; Izquierdo-Hornillos, R

    2000-05-26

    An HPLC separation of a complex mixture containing 13 urinary anabolics and corticoids, and boldenone and bolasterone (synthetic anabolics) has been carried out. The applied optimization method involved the use of binary, ternary and quaternary mobile phases containing acetonitrile, methanol or tetrahydrofuran as organic modifiers. The effect of different reversed-phase packings and temperature on the separation was studied. The optimum separation was achieved by using a water-acetonitrile (60:40, v/v) mobile phase in reversed-phase HPLC at 30 degrees C, allowing the separation of all the analytes in about 24 min. Calibration graphs were obtained using bolasterone or methyltestosterone as internal standards. Detection limits were in the range 0.012-0.107 microg ml(-1). The optimized separation was applied to the analysis, after liquid-liquid extraction, of human urine samples spiked with steroids.

  15. Development and optimization of a miniaturized fiber-optic photoplethysmographic sensor

    NASA Astrophysics Data System (ADS)

    Morley, Aisha; Davenport, John J.; Hickey, Michelle; Phillips, Justin P.

    2017-11-01

    Photoplethysmography (PPG) is a widely used technique for measuring blood oxygen saturation, commonly using an external pulse oximeter applied to a finger, toe, or earlobe. Previous research has demonstrated the utility of direct monitoring of the oxygen saturation of internal organs, using optical fibers to transmit light between the photodiode/light emitting diode and internal site. However, little research into the optimization and standardization of such a probe has yet been carried out. This research establishes the relationship between fiber separation distance and PPG signal, and between fiber core width and PPG signal. An ideal setup is suggested: 1000-μm fibers at a separation distance of 3 to 3.5 mm, which was found to produce signals around 0.35 V in amplitude with a low variation coefficient.

  16. Extended internal standard method for quantitative 1H NMR assisted by chromatography (EIC) for analyte overlapping impurity on 1H NMR spectra.

    PubMed

    Saito, Naoki; Kitamaki, Yuko; Otsuka, Satoko; Yamanaka, Noriko; Nishizaki, Yuzo; Sugimoto, Naoki; Imura, Hisanori; Ihara, Toshihide

    2018-07-01

    We devised a novel extended internal standard method of quantitative 1 H NMR (qNMR) assisted by chromatography (EIC) that accurately quantifies 1 H signal areas of analytes, even when the chemical shifts of the impurity and analyte signals overlap completely. When impurity and analyte signals overlap in the 1 H NMR spectrum but can be separated in a chromatogram, the response ratio of the impurity and an internal standard (IS) can be obtained from the chromatogram. If the response ratio can be converted into the 1 H signal area ratio of the impurity and the IS, the 1 H signal area of the analyte can be evaluated accurately by mathematically correcting the contributions of the 1 H signal area of the impurity overlapping the analyte in the 1 H NMR spectrum. In this study, gas chromatography and liquid chromatography were used. We used 2-chlorophenol and 4-chlorophenol containing phenol as an impurity as examples in which impurity and analyte signals overlap to validate and demonstrate the EIC, respectively. Because the 1 H signals of 2-chlorophenol and phenol can be separated in specific alkaline solutions, 2-chlorophenol is suitable to validate the EIC by comparing analytical value obtained by the EIC with that by only qNMR under the alkaline condition. By the EIC, the purity of 2-chlorophenol was obtained with a relative expanded uncertainty (k = 2) of 0.24%. The purity matched that obtained under the alkaline condition. Furthermore, the EIC was also validated by evaluating the phenol content with the absolute calibration curve method by gas chromatography. Finally, we demonstrated that the EIC was possible to evaluate the purity of 4-chlorophenol, with a relative expanded uncertainty (k = 2) of 0.22%, which was not able to be separated from the 1 H signal of phenol under any condition. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. Simultaneous determination of ascorbic acid and caffeine in commercial soft drinks using reversed-phase ultraperformance liquid chromatography.

    PubMed

    Turak, Fatma; Güzel, Remziye; Dinç, Erdal

    2017-04-01

    A new reversed-phase ultraperformance liquid chromatography method with a photodiode array detector was developed for the quantification of ascorbic acid (AA) and caffeine (CAF) in 11 different commercial drinks consisting of one energy drink and 10 ice tea drinks. Separation of the analyzed AA and CAF with an internal standard, caffeic acid, was performed on a Waters BEH C 18 column (100 mm × 2.1 mm, 1.7 μm i.d.), using a mobile phase consisting of acetonitrile and 0.2M H 3 PO 4 (11:89, v/v) with a flow rate of 0.25 mL/min and an injection volume of 1.0 μL. Calibration graphs for AA and CAF were computed from the peak area ratio of AA/internal standard and CAF/internal standard detected at 244.0 nm and 273.6 nm, respectively. The developed reversed-phase ultraperformance liquid chromatography method was validated by analyzing standard addition samples. The proposed reversed-phase ultraperformance liquid chromatography method gave us successful results for the quantitative analysis of commercial drinks containing AA and CAF substances. Copyright © 2016. Published by Elsevier B.V.

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

    Not Available

    Continuing the tradition established in prior years, this panel encompasses one of the broadest ranges of topics and issues of any panel at the Summer Study. It includes papers addressing all sectors, low-income residential to industrial, and views energy efficiency from many perspectives including programmatic, evaluation, codes, standards, legislation, technical transfer, economic development, and least-cost planning. The papers represent work being performed in most geographic regions of the United States and in the international arena, specifically Thailand, China, Europe, and Scandinavia. This delightful smorgasbord has been organized, based on general content area, into the following eight sessions: (1) new directionsmore » for low-income weatherization; (2) pursuing efficiency through legislation and standards; (3) international perspectives on energy efficiency; (4) technical transfer strategies; (5) government energy policy; (6) commercial codes and standards; (7) innovative programs; and, (8) state-of-the-art review. For these conference proceedings, individual papers are processed separately for the Energy Data Base.« less

  19. Educational Tracking, Inequality and Performance: New Evidence from a Differences-in-Differences Technique

    ERIC Educational Resources Information Center

    Lavrijsen, Jeroen; Nicaise, Ides

    2016-01-01

    One of the important differences between educational systems from different countries is the age at which students are placed into separate tracks. We examined the effects of the age at which tracking occurred on student achievement in a comparative perspective, making use of recent waves of three internationally standardized student assessments…

  20. How noise affects quantum detector tomography

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

    Wang, Q., E-mail: wang@physics.leidenuniv.nl; Renema, J. J.; Exter, M. P.van

    2015-10-07

    We determine the full photon number response of a NbN superconducting nanowire single photon detector via quantum detector tomography, and the results show the separation of linear, effective absorption efficiency from the internal detection efficiencies. In addition, we demonstrate an error budget for the complete quantum characterization of the detector. We find that for short times, the dominant noise source is shot noise, while laser power fluctuations limit the accuracy for longer timescales. The combined standard uncertainty of the internal detection efficiency derived from our measurements is about 2%.

  1. Validation of lipolysis product extraction from aqueous/biological samples, separation and quantification by thin-layer chromatography with flame ionization detection analysis using O-cholesteryl ethylene glycol as a new internal standard.

    PubMed

    Cavalier, Jean-François; Lafont, Dominique; Boullanger, Paul; Houisse, David; Giallo, Jacqueline; Ballester, Jean-Michel; Carrière, Frédéric

    2009-09-11

    A general and easily accessible method for the extraction followed by the simultaneous separation and quantitative determination of triacylglycerols, diacylglycerols, monoacylglycerols and free fatty acids has been improved and optimized based on existing protocols using liquid-phase extraction and thin-layer chromatography coupled to flame ionization detection (TLC/FID Iatroscan). After lipid extraction in the presence of a suitable new synthetic internal standard, namely CholE1, a single elution step using n-heptane/diethyl ether/formic acid (55:45:1, v/v/v) was applied. This method was validated in line with international bioanalytical method validation guidelines using two different matrix systems: purified water and human gastro-intestinal fluid. Overall, the assay was found to have high levels of precision with coefficients of variation ranging from 1.48% to 11.0% and accuracy ranging from -13.3% to +5.79% RE. The confidence limits of the lipid mean recovery rates varied between 89.9% and 104%. This method is therefore highly suitable for quantifying the lipolysis products generated in vitro during the hydrolysis of various fats and oils by digestive lipases, as well as those collected from the gastro-intestinal tract in the course of human clinical studies on lipid digestion.

  2. Nonaqueous capillary electrophoresis of dextromethorphan and its metabolites.

    PubMed

    Pelcová, Marta; Langmajerová, Monika; Cvingráfová, Eliška; Juřica, Jan; Glatz, Zdeněk

    2014-10-01

    This study deals with the nonaqueous capillary electrophoretic separation of dextromethorphan and its metabolites using a methanolic background electrolyte. The optimization of separation conditions was performed in terms of the resolution of dextromethorphan and dextrorphan and the effect of separation temperature, voltage, and the characteristics of the background electrolyte were studied. Complete separation of all analytes was achieved in 40 mM ammonium acetate dissolved in methanol. Hydrodynamic injection was performed at 3 kPa for 4 s. The separation voltage was 20 kV accompanied by a low electric current. The ultraviolet detection was performed at 214 nm, the temperature of the capillary was 25°C. These conditions enabled the separation of four analytes plus the internal standard within 9 min. Further, the developed method was validated in terms of linearity, sensitivity, and repeatability. Rat liver perfusate samples were subjected to the nonaqueous capillary electrophoretic method to illustrate its applicability. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Method development for gypenosides fingerprint by high performance liquid chromatography with diode-array detection and the addition of internal standard.

    PubMed

    Liu, Fang; Ren, Dequan; Guo, De-an; Pan, Yifeng; Zhang, Huzhe; Hu, Ping

    2008-03-01

    In this paper, a new method for liquid chromatographic fingerprint of saponins in Gynostemma pentaphyllum (THUNB.) MAKINO was developed. The G. pentaphyllum powder was defatted by Soxhlet extraction with petroleum ether and then gypenosides were extracted from the residue with methanol by sonicating. Column chromatography with macro pore resin was then used to separate and enrich gypenosides. HPLC fingerprint analysis of gypenosides fraction was performed on a C18 column, with an isocratic elution of 34% acetonitrile for 60 min at 0.8 ml/min, sample injection volume was 20 microl and the wavelength was 203 nm. To cover the lack of standard compounds, the addition of an internal standard of ginsenoside Rb2 was employed in the gypenosides fingerprint profile. The relative retention time (RRT) and relative peak area (RPA) of the gypenosides peaks in the fingerprint were calculated by setting the ginsenoside Rb2 as the marker compound. The relative standard deviation (RSDs) of RRT of five common peaks vs. ginsenoside Rb2 in precision, repeatability and stability test were less than 1%, and the RSDs of RPA were less than 5%. The method validation data proved that the proposed method for the fingerprint with internal standard of G. pentaphyllum saponins is adequate, valid and applicable. Finally, three batches of crude drug samples collected from Shanxi province were tested by following the established method.

  4. Development of liquid chromatographic methods for the determination of phytosterols in Standard Reference Materials containing saw palmetto.

    PubMed

    Bedner, Mary; Schantz, Michele M; Sander, Lane C; Sharpless, Katherine E

    2008-05-23

    Liquid chromatographic (LC) methods using atmospheric pressure chemical ionization/mass spectrometric (APCI-MS) detection were developed for the separation and analysis of the phytosterols campesterol, cycloartenol, lupenone, lupeol, beta-sitosterol, and stigmasterol. Brassicasterol and cholesterol were also included for investigation as internal standards. The methods were used to identify and quantify the phytosterols in each of two Serenoa repens (saw palmetto) Standard Reference Materials (SRMs) developed by the National Institute of Standards and Technology (NIST). Values obtained by LC-MS were compared to those obtained using the more traditional approach of gas chromatography with flame ionization detection. This is the first reported use of LC-MS to determine phytosterols in saw palmetto dietary supplement materials.

  5. Launch COLA Gap Analysis for Protection of the International Space Station

    NASA Astrophysics Data System (ADS)

    Jenkin, Alan B.; McVey, John P.; Peterson, Glenn E.; Sorge, Marlon E.

    2013-08-01

    For launch missions in general, a collision avoidance (COLA) gap exists between the end of the time interval covered by standard launch COLA screening and the time that other spacecraft can clear a collision with the newly launched objects. To address this issue for the International Space Station (ISS), a COLA gap analysis process has been developed. The first part of the process, nodal separation analysis, identifies launch dates and launch window opportunities when the orbit traces of a launched object and the ISS could cross during the COLA gap. The second and newest part of the analysis process, Monte Carlo conjunction probability analysis, is performed closer to the launch dates of concern to reopen some of the launch window opportunities that would be closed by nodal separation analysis alone. Both parts of the process are described and demonstrated on sample missions.

  6. [Simultaneous determination of delta-9-tetrahydrocannabinol cannabidiol and cannabinol in edible oil using ultra performance liquid chromatography-tandem mass spectrometry].

    PubMed

    Zhang, Aizhi; Wang, Quanlin; Mo, Shijie

    2010-11-01

    A method for the simultaneous determination of delta-9-tetrahydrocannabinol (THC), cannabidiol (CBD) and cannabinol (CBN) in edible oil was developed using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The target compounds were extracted with methanol, purified by an LC-Alumina-N solid phase extraction cartridge, separated and detected by the UPLC-MS/MS. Quantitative analysis was corrected by an isotope internal standard method using delta-9-THC-D3 as internal standard. Average recoveries for the target compounds varied from 68.0% to 101.6% with the relative standard deviations ranging from 7.0% to 20.1% at three spiked levels. The limits of detection (LOD) of the method were from 0.06-0.17 microg/kg and the limits of quantification (LOQ) were in the range of 0.20-0.52 microg/kg. The results showed that the method is able to meet the requirements for the simultaneous determination of THC, CBD and CBN in edible oil.

  7. Resource allocation planning with international components

    NASA Technical Reports Server (NTRS)

    Burke, Gene; Durham, Ralph; Leppla, Frank; Porter, David

    1993-01-01

    Dumas, Briggs, Reid and Smith (1989) describe the need for identifying mutually acceptable methodologies for developing standard agreements for the exchange of tracking time or facility use among international components. One possible starting point is the current process used at the Jet Propulsion Laboratory (JPL) in planning the use of tracking resources. While there is a significant promise of better resource utilization by international cooperative agreements, there is a serious challenge to provide convenient user participation given the separate project and network locations. Coordination among users and facility providers will require a more decentralized communication process and a wider variety of automated planning tools to help users find potential exchanges. This paper provides a framework in which international cooperation in the utilization of ground based space communication systems can be facilitated.

  8. Preparative separation of α- and β-santalenes and (Z)-α- and (Z)-β-santalols using silver nitrate-impregnated silica gel medium pressure liquid chromatography and analysis of sandalwood oil.

    PubMed

    Daramwar, Pankaj P; Srivastava, Prabhakar Lal; Priyadarshini, Balaraman; Thulasiram, Hirekodathakallu V

    2012-10-07

    The major sesquiterpene constituents of East-Indian sandalwood oil (Z)-α- and (Z)-β-santalols have shown to be responsible for most of the biological activities and organoleptic properties of sandalwood oil. The work reported here describes the strategic use of medium pressure liquid chromatography (MPLC) for the separation of both α- and β-santalenes and (Z)-α- and (Z)-β-santalols. Silver nitrate impregnated silica gel was used as the stationary phase in MPLC for quantitative separation of α- and β-santalenes and (Z)-α- and (Z)-β-santalols with mobile phases hexane and dichloromethane, respectively. The purities of α-santalene and (Z)-α-santalol obtained were >96%; however, β-santalene and (Z)-β-santalol were obtained with their respective inseparable epi-isomers. Limits of quantification (LoQ) relative to the FID detector were measured for important sesquiterpene alcohols of heartwood oil of S. album using serial dilutions of the standard stock solutions and demonstrated that the quality of the commercial sandalwood oil can be assessed for the content of individual sesquiterpene alcohols regulated by Australian Standard (AS2112-2003), International Organization for Standardization ISO 3518:2002 (E) and European Union (E. U.).

  9. Inductively Coupled Plasma Mass Spectrometry: Sample Analysis of Zirconium and Ruthenium in Metal Organic Frameworks

    DTIC Science & Technology

    2018-02-01

    international proficiency testing sponsored by the Organisation for the Prohibition of Chemical Weapons (The Hague, Netherlands). Traditionally...separate batch of standards at each level for a total of six analyses at each calibration level. Concentrations of the tested calibration levels are...and ruthenium at each calibration level. 11 REFERENCES 1. General Requirements for the Competence of Testing and Calibration Laboratories

  10. Quantitative liquid chromatographic determination of bromadoline and its N-demethylated metabolites in blood, plasma, serum, and urine samples.

    PubMed

    Peng, G W; Sood, V K; Rykert, U M

    1985-03-01

    Bromadoline and its two N-demethylated metabolites were extracted into ether:butyl chloride after the addition of internal standard and basification of the various biological fluids (blood, plasma, serum, and urine). These compounds were then extracted into dilute phosphoric acid from the organic phase and separated on a reversed-phase chromatographic system using a mobile phase containing acetonitrile and a buffer of 1,4-dimethylpiperazine and perchloric acid. The overall absolute extraction recoveries of these compounds were approximately 50-80%. The background interferences from the biological fluids were negligible and allowed quantitative determination of bromadoline and the metabolites at levels as low as 2-5 ng/mL. At mobile phase flow rate of 1 mL/min, the sample components and the internal standard were eluted at the retention times within approximately 7-12 min. The drug- and metabolite-to-internal standard peak height ratios showed excellent linear relationships with their corresponding concentrations. The analytical method showed satisfactory within- and between-run assay precision and accuracy, and has been utilized in the simultaneous determination of bromadoline and its two N-demethylated metabolites in biological fluids collected from humans and from dogs after administration of bromadoline maleate.

  11. Isocratic non-aqueous reversed-phase high-performance liquid chromatographic separation of capsanthin and capsorubin in red peppers (Capsicum annuum L.), paprika and oleoresin.

    PubMed

    Weissenberg, M; Schaeffler, I; Menagem, E; Barzilai, M; Levy, A

    1997-01-03

    A simple, rapid high-performance liquid chromatography method has been devised in order to separate and quantify the xanthophylls capsorubin and capasanthin present in red pepper (Capsicum annuum L.) fruits and preparations made from them (paprika and oleoresin). A reversed-phase isocratic non-aqueous system allows the separation of xanthophylls within a few minutes, with detection at 450 nm, using methyl red as internal standard to locate the various carotenoids and xanthophylls found in plant extracts. The selection of extraction solvents, mild saponification conditions, and chromatographic features is evaluated and discussed. The method is proposed for rapid screening of large plant populations, plant selection, as well as for paprika products and oleoresin, and also for nutrition and quality control studies.

  12. Health care and human rights: against the split duty gambit.

    PubMed

    Sreenivasan, Gopal

    2016-08-01

    There are various grounds on which one may wish to distinguish a right to health care from a right to health. In this article, I review some old grounds before introducing some new grounds. But my central task is to argue that separating a right to health care from a right to health has objectionable consequences. I offer two main objections. The domestic objection is that separating the two rights prevents the state from fulfilling its duty to maximise the health it provides each citizen from its fixed health budget. The international objection is that separating a human right to health care fails the moral requirement that, for any given moral human right, the substance to which any two right-holders are entitled be of an equal standard.

  13. Determination of dapsone in serum and saliva using reversed-phase high-performance liquid chromatography with ultraviolet or electrochemical detection.

    PubMed

    Moncrieff, J

    1994-03-18

    A simple, extractionless method for the determination of dapsone in serum and saliva is described. Reversed-phase high-performance liquid chromatography is used with UV detection at 295 nm or electrochemical detection at 0.7 V. Diazoxide in buffer is the internal standard for UV detection and practolol for electrochemical detection. Sample preparation is minimal with protein precipitation of serum samples whilst saliva samples are simply diluted with addition of an internal standard. Low-level serum and saliva samples are front-cut on-line with a 3 cm laboratory-made precolumn in the loop position on a standard Valco injection valve. Isocratic separation is achieved on a 250 mm x 4.6 mm I.D. stainless-steel Spherisorb S5 ODS-1 column. The mobile phase for high levels of dapsone is acetonitrile-elution buffer (12:88, v/v) at 2 ml/min and a column temperature of 40 degrees C for both serum and saliva separations. For the low-level assays using electrochemical detection and solid-phase clean-up, the mobile phase is acetonitrile-methanol-elution buffer (9:4:87, v/v/v). The UV and electrochemical detection limits are 25 ng/ml and 200 pg/ml, respectively, in both serum and saliva. This simple method is applicable to the routine monitoring of dapsone levels in serum from leprotic patients and electrochemical detection gives a simple, reliable method for the monitoring of trough values in subjects on anti-malarial prophylaxis.

  14. [Rapid determination of volatile organic compounds in workplace air by protable gas chromatography-mass spectrometer].

    PubMed

    Zhu, H B; Su, C J; Tang, H F; Ruan, Z; Liu, D H; Wang, H; Qian, Y L

    2017-10-20

    Objective: To establish a method for rapid determination of 47 volatile organic compounds in the air of workplace using portable gas chromatography - mass spectrometer(GC - MS). Methods: The mixed standard gas with different concentration levels was made by using the static gas distribution method with the high purity nitrogen as dilution gas. The samples were injected into the GC - MS by a hand - held probe. Retention time and characteristic ion were used for qualitative analysis,and the internal standard method was usd for quantitation. Results: The 47 poisonous substances were separated and determined well. The linear range of this method was 0.2 - 16.0 mg/m(3),and the relative standard deviation of 45 volatile ovganic compounds was 3.8% - 15.8%. The average recovery was 79.3% - 119.0%. Conclusion: The method is simple,accurate,sensitive,has good separation effect,short analysis period, can be used for qualitative and quantitative analysis of volatile organic compounds in the workplace, and also supports the rapid identification and detection of occupational hazards.

  15. Quantitative analysis of synthetic dyes in lipstick by micellar electrokinetic capillary chromatography.

    PubMed

    Desiderio, C; Marra, C; Fanali, S

    1998-06-01

    The separation of synthetic dyes, used as color additives in cosmetics, by micellar electrokinetic capillary chromatography (MEKC) is described in this study. The separation of seven dyes, namely eosine, erythrosine, cyanosine, rhodamine B, orange II, chromotrope FB and tartrazine has been achieved in about 3 min in an untreated fused silica capillary containing as background electrolyte a 25 mM tetraborate/phosphate buffer, pH 8.0, and 30 mM sodium dodecyl sulfate. The electrophoretic method exhibits precision and relatively high sensitivity. A detection limit (LOD, signal/noise = 3) in the range of 5-7.5 X 10(-7) M of standard compounds was recorded. Intra-day repeatability of all the studied dye determinations (8 runs) gave the following results (limit values), % standard deviation: 0.24-1.54% for migration time, 0.99-1.24% for corrected peak areas, 0.99-1.24% for corrected peak area ratio (analyte/internal standard) and 1.56-2.74% for peak areas. The optimized method was successfully applied to the analysis of a lipstick sample where eosine and cyanosine were present.

  16. Quantitative mass spectrometric analysis of ropivacaine and bupivacaine in authentic, pharmaceutical and spiked human plasma without chromatographic separation.

    PubMed

    Salama, Nahla N; Wang, Shudong

    2008-05-28

    The present study employs time of flight mass and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL(-1) for both drugs. The correlation coefficient was >or=0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%-102.75% was obtained. The method is accurate (% RE < 5%) and reproducible with intra- and inter-assay precision (RSD% < 8.0%). The quantification limit is 23.8 ng mL(-1) for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs.

  17. Quantitative Mass Spectrometric Analysis of Ropivacaine and Bupivacaine in Authentic, Pharmaceutical and Spiked Human Plasma without Chromatographic Separation

    PubMed Central

    Salama, Nahla N.; Wang, Shudong

    2009-01-01

    The present study employs time of flight mass and bupivacaine in authentic, pharmaceutical and spiked human plasma as well as in the presence of their impurities 2,6-dimethylaniline and alkaline degradation product. The method is based on time of flight electron spray ionization mass spectrometry technique without preliminary chromatographic separation and makes use of bupivacaine as internal standard for ropivacaine, which is used as internal standard for bupivacaine. A linear relationship between drug concentrations and the peak intensity ratio of ions of the analyzed substances is established. The method is linear from 23.8 to 2380.0 ng mL−1 for both drugs. The correlation coefficient was ≥0.996 in authentic and spiked human plasma. The average percentage recoveries in the ranges of 95.39%–102.75% was obtained. The method is accurate (% RE < 5%) and reproducible with intra- and inter-assay precision (RSD% < 8.0%). The quantification limit is 23.8 ng mL−1 for both drugs. The method is not only highly sensitive and selective, but also simple and effective for determination or identification of both drugs in authentic and biological fluids. The method can be applied in purity testing, quality control and stability monitoring for the studied drugs. PMID:19652756

  18. High pressure liquid chromatographic method for the separation and quantitation of water-soluble radiolabeled benzene metabolites

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

    Sabourin, P.J.; Bechtold, W.E.; Henderson, R.F.

    1988-05-01

    The glucuronide and sulfate conjugates of benzene metabolite as well as muconic acid and pre-phenyl- and phenylmercapturic acids were separated by ion-pairing HPLC. The HPLC method developed was suitable for automated analysis of a large number of tissue or excreta samples. p-Nitrophenyl (/sup 14/C)glucuronide was used as an internal standard for quantitation of these water-soluble metabolites. Quantitation was verified by spiking liver tissue with various amounts of phenylsulfate or glucuronides of phenol, catechol, or hydroquinone and analyzing by HPLC. Values determined by HPLC analysis were within 10% of the actual amount with which the liver was spiked. The amount ofmore » metabolite present in urine following exposure to (/sup 3/H)benzene was determined using p-nitrophenyl (/sup 14/C)glucuronide as an internal standard. Phenylsulfate was the major water-soluble metabolite in the urine of F344 rats exposed to 50 ppm (/sup 3/H)benzene for 6 h. Muconic acid and an unknown metabolite which decomposed in acidic media to phenylmercapturic acid were also present. Liver, however, contained a different metabolic profile. This indicates that urinary metabolite profiles may not be a true reflection of what is seen in individual tissues.« less

  19. ANZSoilML: An Australian - New Zealand standard for exchange of soil data

    NASA Astrophysics Data System (ADS)

    Simons, Bruce; Wilson, Peter; Ritchie, Alistair; Cox, Simon

    2013-04-01

    The Australian-New Zealand soil information exchange standard (ANZSoilML) is a GML-based standard designed to allow the discovery, query and delivery of soil and landscape data via standard Open Geospatial Consortium (OGC) Web Feature Services. ANZSoilML modifies the Australian soil exchange standard (OzSoilML), which is based on the Australian Soil Information Transfer and Evaluation System (SITES) database design and exchange protocols, to meet the New Zealand National Soils Database requirements. The most significant change was the removal of the lists of CodeList terms in OzSoilML, which were based on the field methods specified in the 'Australian Soil and Land Survey Field Handbook'. These were replaced with empty CodeLists as placeholders to external vocabularies to allow the use of New Zealand vocabularies without violating the data model. Testing of the use of these separately governed Australian and New Zealand vocabularies has commenced. ANZSoilML attempts to accommodate the proposed International Organization for Standardization ISO/DIS 28258 standard for soil quality. For the most part, ANZSoilML is consistent with the ISO model, although major differences arise as a result of: • The need to specify the properties appropriate for each feature type; • The inclusion of soil-related 'Landscape' features; • Allowing the mapping of soil surfaces, bodies, layers and horizons, independent of the soil profile; • Allowing specifying the relationships between the various soil features; • Specifying soil horizons as specialisations of soil layers; • Removing duplication of features provided by the ISO Observation & Measurements standard. The International Union of Soil Sciences (IUSS) Working Group on Soil Information Standards (WG-SIS) aims to develop, promote and maintain a standard to facilitate the exchange of soils data and information. Developing an international exchange standard that is compatible with existing and emerging national and regional standards is a considerable challenge. ANZSoilML is proposed as a profile of the more generalised SoilML model being progressed through the IUSS Working Group.

  20. Determination of plasma azathioprine and 6-mercaptopurine in patients with rheumatoid arthritis treated with oral azathioprine.

    PubMed

    Liliemark, J; Pettersson, B; Lafolie, P; Zweig, T; Peterson, C

    1990-07-01

    Two specific high-performance liquid chromatography methods for determining plasma concentrations of azathioprine and 6-mercaptopurine after oral administration of azathioprine are presented. It was shown that azathioprine is unstable in the blood samples unless immediately cooled in ice water. The 2-amino analog, guaneran, was used as internal standard for azathioprine, which was extracted from plasma with ethylacetate. A Nucleosil C18 column was used for the separation. The detection limit was 6 nM. For quantification of 6-mercaptopurine, 6-thioguanine was used as internal standard. Plasma was deproteinized with HClO4 and the sample was purified on mercurial cellulose. A Beckman ODS column was used and the detection limit was 5 nM. Pharmacokinetic data from two patients are presented. Unchanged azathioprine was seen until 6 h after an oral dose of 32 mg/m2.

  1. Robust sensor for turbidity measurement from light scattering and absorbing liquids.

    PubMed

    Kontturi, Ville; Turunen, Petri; Uozumi, Jun; Peiponen, Kai-Erik

    2009-12-01

    Internationally standardized turbidity measurements for probing solid particles in liquid are problematic in the case of simultaneous light scattering and absorption. A method and a sensor to determine the turbidity in the presence of light absorption are presented. The developed sensor makes use of the total internal reflection of a laser beam at the liquid-prism interface, and the turbidity is assessed using the concept of laser speckle pattern. Using average filtering in speckle data analyzing the observed dynamic speckle pattern, which is due to light scattering from particles and the static speckle due to stray light of the sensor, can be separated from each other. Good correlation between the standard deviation of dynamic speckle and turbidity value for nonabsorbing and for absorbing liquids was observed. The sensor is suggested, for instance, for the measurement of ill-behaved as well as small-volume turbid liquids in both medicine and process industry.

  2. Assay of free captopril in human plasma as monobromobimane derivative, using RPLC/(+)ESI/MS/MS: validation aspects and bioequivalence evaluation.

    PubMed

    Medvedovici, Andrei; Albu, Florin; Sora, Iuliana Daniela; Udrescu, Stefan; Galaon, Toma; David, Victor

    2009-10-01

    A sensitive method for determination of free captopril as monobromobimane derivative in plasma samples is discussed. The internal standard (IS) was 5-methoxy-1H-benzimidazole-2-thiol. Derivatization with monobromobimane immediately after blood collection and plasma preparation prevents oxidation of captopril to the corresponding disulfide compound and enhances the ionization yield. Consequently, derivatization enhances sample stability and detection sensitivity. Addition of the internal standard was made immediately after plasma preparation. The internal standard was also derivatized by monobromobimane, as it contains a thiol functional group. Preparation of plasma samples containing captopril and IS derivatives was based upon protein precipitation through addition of acetonitrile, in a volumetric ratio 1:2. The reversed-phase liquid chromatographic separation was achieved on a rapid resolution cartridge Zorbax SB-C(18), monitored through positive electrospray ionization and tandem MS detection using the multiple-reaction monitoring mode. Transitions were 408-362 amu for the captopril derivative and 371-260 amu for the internal standard derivative. The kinetics of captopril oxidation to the corresponding disulfide compound in plasma matrix was also studied using the proposed method. A linear log-log calibration was obtained over the concentration interval 2.5-750 ng/mL. A low limit of quantitation in the 2.5 ng/mL range was obtained. The analytical method was fully validated and successfully applied in a three-way, three-period, single-dose (50 mg), block-randomized bioequivalence study for two pharmaceutical formulations (captopril LPH 25 and 50 mg) against the comparator Capoten 50 mg. Copyright (c) 2009 John Wiley & Sons, Ltd.

  3. Exascale computing and big data

    DOE PAGES

    Reed, Daniel A.; Dongarra, Jack

    2015-06-25

    Scientific discovery and engineering innovation requires unifying traditionally separated high-performance computing and big data analytics. The tools and cultures of high-performance computing and big data analytics have diverged, to the detriment of both; unification is essential to address a spectrum of major research domains. The challenges of scale tax our ability to transmit data, compute complicated functions on that data, or store a substantial part of it; new approaches are required to meet these challenges. Finally, the international nature of science demands further development of advanced computer architectures and global standards for processing data, even as international competition complicates themore » openness of the scientific process.« less

  4. Exascale computing and big data

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

    Reed, Daniel A.; Dongarra, Jack

    Scientific discovery and engineering innovation requires unifying traditionally separated high-performance computing and big data analytics. The tools and cultures of high-performance computing and big data analytics have diverged, to the detriment of both; unification is essential to address a spectrum of major research domains. The challenges of scale tax our ability to transmit data, compute complicated functions on that data, or store a substantial part of it; new approaches are required to meet these challenges. Finally, the international nature of science demands further development of advanced computer architectures and global standards for processing data, even as international competition complicates themore » openness of the scientific process.« less

  5. Studies on separation and purification of fission (99)Mo from neutron activated uranium aluminum alloy.

    PubMed

    Rao, Ankita; Kumar Sharma, Abhishek; Kumar, Pradeep; Charyulu, M M; Tomar, B S; Ramakumar, K L

    2014-07-01

    A new method has been developed for separation and purification of fission (99)Mo from neutron activated uranium-aluminum alloy. Alkali dissolution of the irradiated target (100mg) results in aluminum along with (99)Mo and a few fission products passing into solution, while most of the fission products, activation products and uranium remain undissolved. Subsequent purification steps involve precipitation of aluminum as Al(OH)3, iodine as AgI/AgIO3 and molybdenum as Mo-α-benzoin oxime. Ruthenium is separated by volatilization as RuO4 and final purification of (99)Mo was carried out using anion exchange method. The radiochemical yield of fission (99)Mo was found to be >80% and the purity of the product was in conformity with the international pharmacopoeia standards. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Fast Eigensolver for Computing 3D Earth's Normal Modes

    NASA Astrophysics Data System (ADS)

    Shi, J.; De Hoop, M. V.; Li, R.; Xi, Y.; Saad, Y.

    2017-12-01

    We present a novel parallel computational approach to compute Earth's normal modes. We discretize Earth via an unstructured tetrahedral mesh and apply the continuous Galerkin finite element method to the elasto-gravitational system. To resolve the eigenvalue pollution issue, following the analysis separating the seismic point spectrum, we utilize explicitly a representation of the displacement for describing the oscillations of the non-seismic modes in the fluid outer core. Effectively, we separate out the essential spectrum which is naturally related to the Brunt-Väisälä frequency. We introduce two Lanczos approaches with polynomial and rational filtering for solving this generalized eigenvalue problem in prescribed intervals. The polynomial filtering technique only accesses the matrix pair through matrix-vector products and is an ideal candidate for solving three-dimensional large-scale eigenvalue problems. The matrix-free scheme allows us to deal with fluid separation and self-gravitation in an efficient way, while the standard shift-and-invert method typically needs an explicit shifted matrix and its factorization. The rational filtering method converges much faster than the standard shift-and-invert procedure when computing all the eigenvalues inside an interval. Both two Lanczos approaches solve for the internal eigenvalues extremely accurately, comparing with the standard eigensolver. In our computational experiments, we compare our results with the radial earth model benchmark, and visualize the normal modes using vector plots to illustrate the properties of the displacements in different modes.

  7. Determination of fenoterol in human plasma by HPLC with fluorescence detection after derivatization.

    PubMed

    Meineke, Ingolf; Steinmetz, Hannelore; Kramer, Skaidrit; Gleiter, Christoph H

    2002-06-20

    A new method for the determination of fenoterol is described, which uses HPLC separation with fluorescence detection. Dobutamine is employed as an internal standard. The separation was achieved on a short reversed phase column with a mobile phase consisting of water, acetonitrile and methanol. Prior to chromatography both analytes are derivatized with 9-chloroformyl-carbazole. Isolation of the analytes from plasma is carried out by liquid-liquid extraction into 2-butanol after protein precipitation with acetonitrile. The method is capable of estimating fenoterol concentrations in the sub-nanogram per ml range with sufficient accuracy and precision. The determination of fenoterol can now be carried out in the average laboratory without radiolabelled material.

  8. Precise determination of N-acetylcysteine in pharmaceuticals by microchip electrophoresis.

    PubMed

    Rudašová, Marína; Masár, Marián

    2016-01-01

    A novel microchip electrophoresis method for the rapid and high-precision determination of N-acetylcysteine, a pharmaceutically active ingredient, in mucolytics has been developed. Isotachophoresis separations were carried out at pH 6.0 on a microchip with conductivity detection. The methods of external calibration and internal standard were used to evaluate the results. The internal standard method effectively eliminated variations in various working parameters, mainly run-to-run fluctuations of an injected volume. The repeatability and accuracy of N-acetylcysteine determination in all mucolytic preparations tested (Solmucol 90 and 200, and ACC Long 600) were more than satisfactory with the relative standard deviation and relative error values <0.7 and <1.9%, respectively. A recovery range of 99-101% of N-acetylcysteine in the analyzed pharmaceuticals predetermines the proposed method for accurate analysis as well. This work, in general, indicates analytical possibilities of microchip isotachophoresis for the quantitative analysis of simplified samples such as pharmaceuticals that contain the analyte(s) at relatively high concentrations. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Use of the kalamazoo essential elements communication checklist (adapted) in an institutional interpersonal and communication skills curriculum.

    PubMed

    Joyce, Barbara L; Steenbergh, Timothy; Scher, Eric

    2010-06-01

    This study examined the psychometric properties of the Kalamazoo Essential Elements Communication Checklist (Adapted) (KEECC-A), which addresses 7 key elements of physician communication identified in the Kalamazoo Consensus Statement, in a sample of 135 residents in multiple specialties at a large urban medical center in 2008-2009. The KEECC-A was used by residents, standardized patients, and faculty as the assessment tool in a broader institutional curriculum initiative. Three separate KEECC-A scores (self-ratings, faculty ratings, and standardized patient ratings) were calculated for each resident to assess the internal consistency and factor structure of the checklist. In addition, we analyzed KEECC-A ratings by gender and US versus international medical graduates, and collected American Board of Internal Medicine Patient Satisfaction Questionnaire (PSQ) scores for a subsample of internal medicine residents (n  =  28) to examine the relationship between this measure and the KEECC-A ratings to provide evidence of convergent validity. The KEECC-A ratings generated by faculty, standardized patients, and the residents themselves demonstrated a high degree of internal consistency. Factor analyses of the 3 different sets of KEECC-A ratings produced a consistent single-factor structure. We could not examine the relationship between KEECC-A and the PSQ because of substantial range restriction in PSQ scores. No differences were seen in the communication scores of men versus women. Faculty rated US graduates significantly higher than international medical graduates. Our study provides evidence for the reliability and validity of the KEECC-A as a measure of physician communication skills. The KEECC-A appears to be a psychometrically sound, user-friendly communication tool, linked to an expert consensus statement, that can be quickly and accurately completed by multiple raters across diverse specialties.

  10. International trade standards for commodities and products derived from animals: the need for a system that integrates food safety and animal disease risk management.

    PubMed

    Thomson, G R; Penrith, M-L; Atkinson, M W; Thalwitzer, S; Mancuso, A; Atkinson, S J; Osofsky, S A

    2013-12-01

    A case is made for greater emphasis to be placed on value chain management as an alternative to geographically based disease risk mitigation for trade in commodities and products derived from animals. The geographic approach is dependent upon achievement of freedom in countries or zones from infectious agents that cause so-called transboundary animal diseases, while value chain-based risk management depends upon mitigation of animal disease hazards potentially associated with specific commodities or products irrespective of the locality of production. This commodity-specific approach is founded on the same principles upon which international food safety standards are based, viz. hazard analysis critical control points (HACCP). Broader acceptance of a value chain approach enables animal disease risk management to be combined with food safety management by the integration of commodity-based trade and HACCP methodologies and thereby facilitates 'farm to fork' quality assurance. The latter is increasingly recognized as indispensable to food safety assurance and is therefore a pre-condition to safe trade. The biological principles upon which HACCP and commodity-based trade are based are essentially identical, potentially simplifying sanitary control in contrast to current separate international sanitary standards for food safety and animal disease risks that are difficult to reconcile. A value chain approach would not only enable more effective integration of food safety and animal disease risk management of foodstuffs derived from animals but would also ameliorate adverse environmental and associated socio-economic consequences of current sanitary standards based on the geographic distribution of animal infections. This is especially the case where vast veterinary cordon fencing systems are relied upon to separate livestock and wildlife as is the case in much of southern Africa. A value chain approach would thus be particularly beneficial to under-developed regions of the world such as southern Africa specifically and sub-Saharan Africa more generally where it would reduce incompatibility between attempts to expand and commercialize livestock production and the need to conserve the subcontinent's unparalleled wildlife and wilderness resources. © 2013 Blackwell Verlag GmbH.

  11. Reduction of Solvent Effect in Reverse Phase Gradient Elution LC-ICP-MS

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

    Sullivan, Patrick Allen

    2005-12-17

    Quantification in liquid chromatography (LC) is becoming very important as more researchers are using LC, not as an analytical tool itself, but as a sample introduction system for other analytical instruments. The ability of LC instrumentation to quickly separate a wide variety of compounds makes it ideal for analysis of complex mixtures. For elemental speciation, LC is joined with inductively coupled plasma mass spectrometry (ICP-MS) to separate and detect metal-containing, organic compounds in complex mixtures, such as biological samples. Often, the solvent gradients required to perform complex separations will cause matrix effects within the plasma. This limits the sensitivity ofmore » the ICP-MS and the quantification methods available for use in such analyses. Traditionally, isotope dilution has been the method of choice for LC-ICP-MS quantification. The use of naturally abundant isotopes of a single element in quantification corrects for most of the effects that LC solvent gradients produce within the plasma. However, not all elements of interest in speciation studies have multiple naturally occurring isotopes; and polyatomic interferences for a given isotope can develop within the plasma, depending on the solvent matrix. This is the case for reverse phase LC separations, where increasing amounts of organic solvent are required. For such separations, an alternative to isotope dilution for quantification would be is needed. To this end, a new method was developed using the Apex-Q desolvation system (ESI, Omaha, NE) to couple LC instrumentation with an ICP-MS device. The desolvation power of the system allowed greater concentrations of methanol to be introduced to the plasma prior to destabilization than with direct methanol injection into the plasma. Studies were performed, using simulated and actual linear methanol gradients, to find analyte-internal standard (AIS) pairs whose ratio remains consistent (deviations {+-} 10%) over methanol concentration ranges of 5%-35% (simulated) and 8%-32% (actual). Quadrupole (low resolution) and sector field (high resolution) ICP-MS instrumentation were utilized in these studies. Once an AIS pair is determined, quantification studies can be performed. First, an analysis is performed by adding both elements of the AIS pair post-column while performing the gradient elution without sample injection. A comparison of the ratio of the measured intensities to the atomic ratio of the two standards is used to determine a correction factor that can be used to account for the matrix effects caused by the mobile phase. Then, organic and/or biological molecules containing one of the two elements in the AIS pair are injected into the LC column. A gradient method is used to vary the methanol-water mixture in the mobile phase and to separate out the compounds in a given sample. A standard solution of the second ion in the AIS pair is added continuously post-column. By comparing the ratio of the measured intensities to the atomic ratio of the eluting compound and internal standard, the concentration of the injected compound can be determined.« less

  12. 40 CFR 61.347 - Standards: Oil-water separators.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 8 2010-07-01 2010-07-01 false Standards: Oil-water separators. 61.347... Waste Operations § 61.347 Standards: Oil-water separators. (a) Except as provided in § 61.352 of this subpart, the owner or operator shall meet the following standards for each oil-water separator in which...

  13. 40 CFR 61.347 - Standards: Oil-water separators.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 8 2011-07-01 2011-07-01 false Standards: Oil-water separators. 61.347... Waste Operations § 61.347 Standards: Oil-water separators. (a) Except as provided in § 61.352 of this subpart, the owner or operator shall meet the following standards for each oil-water separator in which...

  14. 40 CFR 61.347 - Standards: Oil-water separators.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 9 2013-07-01 2013-07-01 false Standards: Oil-water separators. 61.347... Waste Operations § 61.347 Standards: Oil-water separators. (a) Except as provided in § 61.352 of this subpart, the owner or operator shall meet the following standards for each oil-water separator in which...

  15. Uncertainty Analysis for Angle Calibrations Using Circle Closure

    PubMed Central

    Estler, W. Tyler

    1998-01-01

    We analyze two types of full-circle angle calibrations: a simple closure in which a single set of unknown angular segments is sequentially compared with an unknown reference angle, and a dual closure in which two divided circles are simultaneously calibrated by intercomparison. In each case, the constraint of circle closure provides auxiliary information that (1) enables a complete calibration process without reference to separately calibrated reference artifacts, and (2) serves to reduce measurement uncertainty. We derive closed-form expressions for the combined standard uncertainties of angle calibrations, following guidelines published by the International Organization for Standardization (ISO) and NIST. The analysis includes methods for the quantitative evaluation of the standard uncertainty of small angle measurement using electronic autocollimators, including the effects of calibration uncertainty and air turbulence. PMID:28009359

  16. Wake vortex separation standards : analysis methods

    DOT National Transportation Integrated Search

    1997-01-01

    Wake vortex separation standards are used to prevent hazardous wake vortex encounters. A "safe" separation model can be used to assess the safety of proposed changes in the standards. A safe separation model can be derived from an encounter hazard mo...

  17. Analysis of pilocarpine and its trans epimer, isopilocarpine, by capillary electrophoresis.

    PubMed

    Baeyens, W; Weiss, G; Van Der Weken, G; Van Den Bossche, W

    1993-05-28

    Capillary zone electrophoresis was used for the separation of pilocarpine from its epimer, isopilocarpine, using coated fused-silica capillaries of 20 cm x 25 microm I.D., 8 kV running voltage, migration buffer of 0.1 M sodium dihydrogenphosphate pH 8, detection at 217 nm and injection by electromigration. Injections of aqueous, acid and basic solutions were compared. Linearity of the signal for pilocarpine hydrochloride up to 200 microg ml(-1) in 0.05 M hydrochloric acid was obtained, using naphazoline nitrate as internal standard. Optimization of migration buffer pH using coated silica capillaries of 50 cm x 50 microm I.D. showed that at pH 6.9 pilocarpine can be separated from ++isopilocarpine. Inclusion of beta-cyclodextrin in the buffer allows full baseline separation of both epimers. The method was applied to the analysis of a commercial ophthalmic pilocarpine solution.

  18. Separation and quantitation of three acidic herbicide residues in tobacco and soil by dispersive solid-phase extraction and UPLC-MS/MS.

    PubMed

    Xiong, Wei; Tao, Xiaoqiu; Pang, Su; Yang, Xue; Tang, GangLing; Bian, Zhaoyang

    2014-01-01

    A method for the determination of three acidic herbicides, dicamba, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in tobacco and soil has been developed based on the use of liquid-liquid extraction and dispersive solid-phase extraction (dispersive-SPE) followed by UPLC-MS/MS. Two percentage of (v/v) formic acid in acetonitrile as the extraction helped partitioning of analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using primary secondary amine as selective sorbents. Quantitative analysis was done in the multiple-reaction monitoring mode using stable isotope-labeled internal standards for each compound. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision. The total analysis time was <4 min. The linear range of the method was from 1 to 100 ng mL(-1) with a limit of detection of each herbicide varied from 0.012 to 0.126 ng g(-1). The proposed method is faster, more sensitive and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  19. Statistical performance of image cytometry for DNA, lipids, cytokeratin, & CD45 in a model system for circulation tumor cell detection.

    PubMed

    Futia, Gregory L; Schlaepfer, Isabel R; Qamar, Lubna; Behbakht, Kian; Gibson, Emily A

    2017-07-01

    Detection of circulating tumor cells (CTCs) in a blood sample is limited by the sensitivity and specificity of the biomarker panel used to identify CTCs over other blood cells. In this work, we present Bayesian theory that shows how test sensitivity and specificity set the rarity of cell that a test can detect. We perform our calculation of sensitivity and specificity on our image cytometry biomarker panel by testing on pure disease positive (D + ) populations (MCF7 cells) and pure disease negative populations (D - ) (leukocytes). In this system, we performed multi-channel confocal fluorescence microscopy to image biomarkers of DNA, lipids, CD45, and Cytokeratin. Using custom software, we segmented our confocal images into regions of interest consisting of individual cells and computed the image metrics of total signal, second spatial moment, spatial frequency second moment, and the product of the spatial-spatial frequency moments. We present our analysis of these 16 features. The best performing of the 16 features produced an average separation of three standard deviations between D + and D - and an average detectable rarity of ∼1 in 200. We performed multivariable regression and feature selection to combine multiple features for increased performance and showed an average separation of seven standard deviations between the D + and D - populations making our average detectable rarity of ∼1 in 480. Histograms and receiver operating characteristics (ROC) curves for these features and regressions are presented. We conclude that simple regression analysis holds promise to further improve the separation of rare cells in cytometry applications. © 2017 International Society for Advancement of Cytometry. © 2017 International Society for Advancement of Cytometry.

  20. A modified beam-to-earth transformation to measure short-wavelength internal waves with an acoustic Doppler current profiler

    USGS Publications Warehouse

    Scotti, A.; Butman, B.; Beardsley, R.C.; Alexander, P.S.; Anderson, S.

    2005-01-01

    The algorithm used to transform velocity signals from beam coordinates to earth coordinates in an acoustic Doppler current profiler (ADCP) relies on the assumption that the currents are uniform over the horizontal distance separating the beams. This condition may be violated by (nonlinear) internal waves, which can have wavelengths as small as 100-200 m. In this case, the standard algorithm combines velocities measured at different phases of a wave and produces horizontal velocities that increasingly differ from true velocities with distance from the ADCP. Observations made in Massachusetts Bay show that currents measured with a bottom-mounted upward-looking ADCP during periods when short-wavelength internal waves are present differ significantly from currents measured by point current meters, except very close to the instrument. These periods are flagged with high error velocities by the standard ADCP algorithm. In this paper measurements from the four spatially diverging beams and the backscatter intensity signal are used to calculate the propagation direction and celerity of the internal waves. Once this information is known, a modified beam-to-earth transformation that combines appropriately lagged beam measurements can be used to obtain current estimates in earth coordinates that compare well with pointwise measurements. ?? 2005 American Meteorological Society.

  1. Amide proton transfer imaging of brain tumors using a self-corrected 3D fast spin-echo dixon method: Comparison With separate B0 correction.

    PubMed

    Togao, Osamu; Keupp, Jochen; Hiwatashi, Akio; Yamashita, Koji; Kikuchi, Kazufumi; Yoneyama, Masami; Honda, Hiroshi

    2017-06-01

    To assess the quantitative performance of three-dimensional (3D) fast spin-echo (FSE) Dixon amide proton transfer (APT) imaging of brain tumors compared with B 0 correction with separate mapping methods. Twenty-two patients with brain tumors (54.2 ± 18.7 years old, 12 males and 10 females) were scanned at 3 Tesla (T). Z-spectra were obtained at seven different frequency offsets at ±3.1 ppm, ± 3.5 ppm, ± 3.9 ppm, and -1560 ppm. The scan was repeated three times at +3.5 ppm with echo shifts for Dixon B 0 mapping. The APT image corrected by a three-point Dixon-type B 0 map from the same scan (3D-Dixon) or a separate B 0 map (2D-separate and 3D-separate), and an uncorrected APT image (3D-uncorrected) were generated. We compared the APT-weighted signals within a tumor obtained with each 3D method with those obtained with 2D-separate as a reference standard. Excellent agreements and correlations with the 2D-separate were obtained by the 3D-Dixon method for both mean (ICC = 0.964, r = 0.93, P < 0.0001) and 90th-percentile (ICC = 0.972, r = 0.95, P < 0.0001) APT-weighted signals. These agreements and correlations for 3D-Dixon were better than those obtained by the 3D-uncorrected and 3D-separate methods. The 3D FSE Dixon APT method with intrinsic B 0 correction offers a quantitative performance that is similar to that of established two-dimensional (2D) methods. Magn Reson Med 77:2272-2279, 2017. © 2016 International Society for Magnetic Resonance in Medicine. © 2016 International Society for Magnetic Resonance in Medicine.

  2. NREL/NASA Internal Short-Circuit Instigator in Lithium Ion Cells

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

    Keyser, Matthew; Long, Dirk; Pesaran, Ahmad

    Lithium-ion cells provide the highest specific energy (>280 Wh/kg) and energy density (>600 Wh/L) rechargeable battery building block to date with the longest life. Electrode/electrolyte thermal instability and flammability of the electrolyte of Li-ion cells make them prone to catastrophic thermal runaway under some rare internal short circuit conditions. Despite extensive QC/QA, standardized industry safety testing, and over 18 years of manufacturing experience, major recalls have taken place and incidents still occur. Many safety incidents that take place in the field originate due to an internal short that was not detectable or predictable at the point of manufacture. The Internalmore » Short-Circuit Instigator can be used to study types of separators, non-flammable electrolytes, electrolyte additives, fusible tabs, propagation studies, and gas generation within a cell.« less

  3. An ultrahigh-performance liquid chromatography method with electrospray ionization tandem mass spectrometry for simultaneous quantification of five phytohormones in medicinal plant Glycyrrhiza uralensis under abscisic acid stress.

    PubMed

    Xiang, Yu; Song, Xiaona; Qiao, Jing; Zang, Yimei; Li, Yanpeng; Liu, Yong; Liu, Chunsheng

    2015-07-01

    An efficient simplified method was developed to determine multiple classes of phytohormones simultaneously in the medicinal plant Glycyrrhiza uralensis. Ultrahigh-performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC/ESI-MS/MS) with multiple reaction monitoring (MRM) in negative mode was used for quantification. The five studied phytohormones are gibberellic acid (GA3), abscisic acid (ABA), jasmonic acid (JA), indole-3-acetic acid, and salicylic acid (SA). Only 100 mg of fresh leaves was needed, with one purification step based on C18 solid-phase extraction. Cinnamic acid was chosen as the internal standard instead of isotope-labeled internal standards. Under the optimized conditions, the five phytohormones with internal standard were separated within 4 min, with good linearities and high sensitivity. The validated method was applied to monitor the spatial and temporal changes of the five phytohormones in G. uralensis under ABA stress. The levels of GA3, ABA, JA, and SA in leaves of G. uralensis were increased at different times and with different tendencies in the reported stress mode. These changes in phytohormone levels are discussed in the context of a possible feedback regulation mechanism. Understanding this mechanism will provide a good chance of revealing the mutual interplay between different biosynthetic routes, which could further help elucidate the mechanisms of effective composition accumulation in medicinal plants.

  4. Separation analysis of macrolide antibiotics with good performance on a positively charged C18HCE column.

    PubMed

    Wei, Jie; Shen, Aijin; Yan, Jingyu; Jin, Gaowa; Yang, Bingcheng; Guo, Zhimou; Zhang, Feifang; Liang, Xinmiao

    2016-03-01

    The separation of basic macrolide antibiotics suffers from peak tailing and poor efficiency on traditional silica-based reversed-phase liquid chromatography columns. In this work, a C18HCE column with positively charged surface was applied to the separation of macrolides. Compared with an Acquity BEH C18 column, the C18HCE column exhibited superior performance in the aspect of peak shape and separation efficiency. The screening of mobile phase additives including formic acid, acetic acid and ammonium formate indicated that formic acid was preferable for providing symmetrical peak shapes. Moreover, the influence of formic acid content was investigated. Analysis speed and mass spectrometry compatibility were also taken into account when optimizing the separation conditions for liquid chromatography coupled with tandem mass spectrometry. The developed method was successfully utilized for the determination of macrolide residues in a honey sample. Azithromycin was chosen as the internal standard for the quantitation of spiramycin and tilmicosin, while roxithromycin was used for erythromycin, tylosin, clarithromycin, josamycin and acetylisovaleryltylosin. Good correlation coefficients (r(2) > 0.9938) for all macrolides were obtained. The intra-day and inter-day recoveries were 73.7-134.7% and 80.7-119.7% with relative standard deviations of 2.5-8.0% and 3.9-16.1%, respectively. Outstanding sensitivity with limits of quantitation (S/N ≥ 10) of 0.02-1 μg/kg and limits of detection (S/N ≥ 3) of 0.01-0.5 μg/kg were achieved. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Standardization of reliability reporting for cochlear implants: an interim report.

    PubMed

    Backous, Douglas D; Watson, Stacey D

    2007-04-01

    To propose a standard definition of "out of specification" for cochlear implants and a paradigm for inclusion of category C of the ISO standard 5841-2:2000 for reporting in cumulative survival statistics. A standard definition of "out of specification" and consistent reporting by manufacturers of cochlear implants will create a fair and consistent representation of cumulative survival. This will allow discernment of differences between manufacturers for reliability and for detection of trends in reliability between model types from the same manufacturer. Three separate meetings with representatives of the three manufacturers of cochlear implants marketed in the United States were staged over a 13-mo period. Standard questions, created by the authors, were addressed by each representative to determine the current state of device reliability reporting. Results were presented to clinicians at the William House Cochlear Implant study Group and the Implantable devices sub-committee of the American Academy of Otolaryngology (2004, 2005) and at the 8th International Cochlear Implant Conference (2004) for feedback. After assimilation of feedback by all parties, the standard was written and reviewed by representatives from each manufacturer for accuracy of data. A complaint-driven standard was developed. A "cochlear implant" as an internal device placed and skin closed in surgery. An internal device is "out of specification" when one or more technical characteristics is outside the limits of normal function and results in explantation or non-use by the patient." Children will be reported separately from adults, each model of device will be reported on annually, a minimum of 200 devices must be in each model group for Cumulative Survival Reporting (CSR). Confidence limits are set at 95%. Explants will be determined to be "biological" or "technical." Technical explants are included in CSR reports. Devices failing to meet specifications set by the manufacturer, not in use but still in situ due to patient choice not to be re-implanted are considered category C and included in CSR reports. Implants that cannot be classified at explant are placed in an "under investigation" category while evaluation is completed. If no classification is made by 6 months, these devices will be included in the CSR report. Notification to the implant center regarding "in" or "out of specification" will be made within 60 d of the explant arriving at the manufacturer with final root cause of failure reported to centers when complete. Information will be passed on to patients by members of the implant team. A standardized form will be created to provide the manufacturers with necessary patient information to guide reliability analysis, including performance after re-implant. The standard for reliability reporting described in this paper improves patient care by presenting data which are understandable to clinicians delivering cochlear implant services. It fosters fair and accurate reporting without discriminating or granting perceived advantage to any manufacturer. This standard provides a basis for reporting research related to or including device reliability in the medical literature.

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

    Lee, Gyeong Won; Shim, Jong-In; Shin, Dong-Soo, E-mail: dshin@hanyang.ac.kr

    While there have been many discussions on the standard Si pn-diodes, little attention has been paid and confusion still arises on the ideality factor of the radiative recombination current in semiconductor light-emitting diodes (LEDs). In this letter, we theoretically demonstrate and experimentally confirm by using blue and infrared semiconductor LEDs that the ideality factor of the radiative recombination current is unity especially for low-current-density ranges. We utilize the data of internal quantum efficiency measured by the temperature-dependent electroluminescence to separate the radiative current component from the total current.

  7. 40 CFR 60.692-3 - Standards: Oil-water separators.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 6 2010-07-01 2010-07-01 false Standards: Oil-water separators. 60.692... Emissions From Petroleum Refinery Wastewater Systems § 60.692-3 Standards: Oil-water separators. (a) Each oil-water separator tank, slop oil tank, storage vessel, or other auxiliary equipment subject to the...

  8. 40 CFR 60.692-3 - Standards: Oil-water separators.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 7 2013-07-01 2013-07-01 false Standards: Oil-water separators. 60.692... Emissions From Petroleum Refinery Wastewater Systems § 60.692-3 Standards: Oil-water separators. (a) Each oil-water separator tank, slop oil tank, storage vessel, or other auxiliary equipment subject to the...

  9. 40 CFR 60.692-3 - Standards: Oil-water separators.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 7 2014-07-01 2014-07-01 false Standards: Oil-water separators. 60.692... Emissions From Petroleum Refinery Wastewater Systems § 60.692-3 Standards: Oil-water separators. (a) Each oil-water separator tank, slop oil tank, storage vessel, or other auxiliary equipment subject to the...

  10. Element fracture technique for hypervelocity impact simulation

    NASA Astrophysics Data System (ADS)

    Zhang, Xiao-tian; Li, Xiao-gang; Liu, Tao; Jia, Guang-hui

    2015-05-01

    Hypervelocity impact dynamics is the theoretical support of spacecraft shielding against space debris. The numerical simulation has become an important approach for obtaining the ballistic limits of the spacecraft shields. Currently, the most widely used algorithm for hypervelocity impact is the smoothed particle hydrodynamics (SPH). Although the finite element method (FEM) is widely used in fracture mechanics and low-velocity impacts, the standard FEM can hardly simulate the debris cloud generated by hypervelocity impact. This paper presents a successful application of the node-separation technique for hypervelocity impact debris cloud simulation. The node-separation technique assigns individual/coincident nodes for the adjacent elements, and it applies constraints to the coincident node sets in the modeling step. In the explicit iteration, the cracks are generated by releasing the constrained node sets that meet the fracture criterion. Additionally, the distorted elements are identified from two aspects - self-piercing and phase change - and are deleted so that the constitutive computation can continue. FEM with the node-separation technique is used for thin-wall hypervelocity impact simulations. The internal structures of the debris cloud in the simulation output are compared with that in the test X-ray graphs under different material fracture criteria. It shows that the pressure criterion is more appropriate for hypervelocity impact. The internal structures of the debris cloud are also simulated and compared under different thickness-to-diameter ratios (t/D). The simulation outputs show the same spall pattern with the tests. Finally, the triple-plate impact case is simulated with node-separation FEM.

  11. 26 CFR 1.414(r)-3 - Separate line of business.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 26 Internal Revenue 5 2013-04-01 2013-04-01 false Separate line of business. 1.414(r)-3 Section 1.414(r)-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES (CONTINUED) Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-3 Separate...

  12. 26 CFR 1.414(r)-3 - Separate line of business.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 5 2011-04-01 2011-04-01 false Separate line of business. 1.414(r)-3 Section 1.414(r)-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES (CONTINUED) Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-3 Separate...

  13. 26 CFR 1.414(r)-3 - Separate line of business.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 26 Internal Revenue 5 2012-04-01 2011-04-01 true Separate line of business. 1.414(r)-3 Section 1.414(r)-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES (CONTINUED) Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-3 Separate...

  14. 26 CFR 1.414(r)-10 - Separate application of section 129(d)(8). [Reserved

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 5 2010-04-01 2010-04-01 false Separate application of section 129(d)(8). [Reserved] 1.414(r)-10 Section 1.414(r)-10 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE.... § 1.414(r)-10 Separate application of section 129(d)(8). [Reserved] ...

  15. 26 CFR 1.414(r)-3 - Separate line of business.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 26 Internal Revenue 5 2014-04-01 2014-04-01 false Separate line of business. 1.414(r)-3 Section 1.414(r)-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES (CONTINUED) Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-3 Separate...

  16. A rapid method for quantification of 242Pu in urine using extraction chromatography and ICP-MS

    DOE PAGES

    Gallardo, Athena Marie; Than, Chit; Wong, Carolyn; ...

    2017-01-01

    Occupational exposure to plutonium is generally monitored through analysis of urine samples. Typically, plutonium is separated from the sample and other actinides, and the concentration is determined using alpha spectroscopy. Current methods for separations and analysis are lengthy and require long count times. A new method for monitoring occupational exposure levels of plutonium has been developed, which requires fewer steps and overall less time than the alpha spectroscopy method. In this method, the urine is acidified, and a 239Pu internal standard is added. The urine is digested in a microwave oven, and plutonium is separated using an Eichrom TRU Resinmore » column. The plutonium is eluted, and the eluant is injected directly into the Inductively Coupled Plasma–Mass Spectrometer (ICP-MS). Compared to a direct “dilute and shoot” method, a 30-fold improvement in sensitivity is achieved. This method was validated by analyzing several batches of spiked samples. Based on these analyses, a combined standard uncertainty plot, which relates uncertainty to concentration, was produced. As a result, the MDA 95 was calculated to be 7.0 × 10 –7 μg L –1, and the Lc95 was calculated to be 3.5 × 10 –7 μg L –1 for this method.« less

  17. Enabling international adoption of LOINC through translation

    PubMed Central

    Vreeman, Daniel J.; Chiaravalloti, Maria Teresa; Hook, John; McDonald, Clement J.

    2012-01-01

    Interoperable health information exchange depends on adoption of terminology standards, but international use of such standards can be challenging because of language differences between local concept names and the standard terminology. To address this important barrier, we describe the evolution of an efficient process for constructing translations of LOINC terms names, the foreign language functions in RELMA, and the current state of translations in LOINC. We also present the development of the Italian translation to illustrate how translation is enabling adoption in international contexts. We built a tool that finds the unique list of LOINC Parts that make up a given set of LOINC terms. This list enables translation of smaller pieces like the core component “hepatitis c virus” separately from all the suffixes that could appear with it, such “Ab.IgG”, “DNA”, and “RNA”. We built another tool that generates a translation of a full LOINC name from all of these atomic pieces. As of version 2.36 (June 2011), LOINC terms have been translated into 9 languages from 15 linguistic variants other than its native English. The five largest linguistic variants have all used the Part-based translation mechanism. However, even with efficient tools and processes, translation of standard terminology is a complex undertaking. Two of the prominent linguistic challenges that translators have faced include: the approach to handling acronyms and abbreviations, and the differences in linguistic syntax (e.g. word order) between languages. LOINC’s open and customizable approach has enabled many different groups to create translations that met their needs and matched their resources. Distributing the standard and its many language translations at no cost worldwide accelerates LOINC adoption globally, and is an important enabler of interoperable health information exchange PMID:22285984

  18. Trajectories of Internalizing, Externalizing, and Grades for Children Who Have and Have Not Experienced Their Parents' Divorce or Separation

    PubMed Central

    Lansford, Jennifer E.; Malone, Patrick S.; Castellino, Domini R.; Dodge, Kenneth A.; Pettit, Gregory S.; Bates, John E.

    2009-01-01

    This study examined whether the occurrence and timing of parental separation or divorce was related to trajectories of academic grades and mother- and teacher-reported internalizing and externalizing problems. The authors used hierarchical linear models to estimate trajectories for children who did and did not experience their parents' divorce or separation in kindergarten through 10th grade (N = 194). A novel approach to analyzing the timing of divorce/separation was adopted, and trajectories were estimated from 1 year prior to the divorce/separation to 3 years after the event. Results suggest that early parental divorce/separation is more negatively related to trajectories of internalizing and externalizing problems than is later divorce/separation, whereas later divorce/separation is more negatively related to grades. One implication of these findings is that children may benefit most from interventions focused on preventing internalizing and externalizing problems, whereas adolescents may benefit most from interventions focused on promoting academic achievement. PMID:16756405

  19. Trajectories of internalizing, externalizing, and grades for children who have and have not experienced their parents' divorce or separation.

    PubMed

    Lansford, Jennifer E; Malone, Patrick S; Castellino, Domini R; Dodge, Kenneth A; Pettit, Gregory S; Bates, John E

    2006-06-01

    This study examined whether the occurrence and timing of parental separation or divorce was related to trajectories of academic grades and mother- and teacher-reported internalizing and externalizing problems. The authors used hierarchical linear models to estimate trajectories for children who did and did not experience their parents' divorce or separation in kindergarten through 10th grade (N = 194). A novel approach to analyzing the timing of divorce/separation was adopted, and trajectories were estimated from 1 year prior to the divorce/separation to 3 years after the event. Results suggest that early parental divorce/separation is more negatively related to trajectories of internalizing and externalizing problems than is later divorce/separation, whereas later divorce/separation is more negatively related to grades. One implication of these findings is that children may benefit most from interventions focused on preventing internalizing and externalizing problems, whereas adolescents may benefit most from interventions focused on promoting academic achievement. ((c) 2006 APA, all rights reserved).

  20. Potential GPRS 900/180-MHz and WCDMA 1900-MHz interference to medical devices.

    PubMed

    Iskra, Steve; Thomas, Barry W; McKenzie, Ray; Rowley, Jack

    2007-10-01

    This study compared the potential for interference to medical devices from radio frequency (RF) fields radiated by GSM 900/1800-MHz, general packet radio service (GPRS) 900/1800-MHz, and wideband code division multiple access (WCDMA) 1900-MHz handsets. The study used a balanced half-wave dipole antenna, which was energized with a signal at the standard power level for each technology, and then brought towards the medical device while noting the distance at which interference became apparent. Additional testing was performed with signals that comply with the requirements of the international immunity standard to RF fields, IEC 61000-4-3. The testing provides a sense of the overall interference impact that GPRS and WCDMA (frequency division duplex) may have, relative to current mobile technologies, and to the internationally recognized standard for radiated RF immunity. Ten medical devices were tested: two pulse oximeters, a blood pressure monitor, a patient monitor, a humidifier, three models of cardiac defibrillator, and two models of infusion pump. Our conclusion from this and a related study on consumer devices is that WCDMA handsets are unlikely to be a significant interference threat to medical electronics at typical separation distances.

  1. Optimized determination method for trans-10-hydroxy-2-decenoic acid content in royal jelly by high-performance liquid chromatography with an internal standard.

    PubMed

    Zhou, Jinhui; Xue, Xiaofeng; Li, Yi; Zhang, Jinzhen; Zhao, Jing

    2007-01-01

    An optimized reversed-phase high-performance liquid chromatography method was developed to detect the trans-10-hydroxy-2-decenoic acid (10-HDA) content in royal jelly cream and lyophilized powder. The sample was extracted using absolute ethanol. Chromatographic separation of 10-HDA and methyl 4-hydroxybenzoate as the internal standard was performed on a Nova-pak C18 column. The average recoveries were 95.0-99.2% (n = 5) with relative standard deviation (RSD) values of 1.3-2.1% for royal jelly cream and 98.0-100.0% (n = 5) with RSD values of 1.6-3.0% for lyophilized powder, respectively. The limits of detection and quantitation were 0.5 and 1.5 mg/kg, respectively, for both royal jelly cream and lyophilized powder. The method was validated for the determination of practical royal jelly products. The concentration of 10-HDA ranged from 1.26 to 2.21% for pure royal jelly cream samples and 3.01 to 6.19% for royal jelly lyophilized powder samples. For 30 royal jelly products, the 10-HDA content varied from not detectable to 0.98%.

  2. Quantitative determination of rocuronium in human plasma by liquid chromatography-electrospray ionization mass spectrometry.

    PubMed

    Farenc, C; Enjalbal, C; Sanchez, P; Bressolle, F; Audran, M; Martinez, J; Aubagnac, J L

    2001-02-23

    Liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) was used for the quantification of the neuromuscular blocking agent rocuronium in human plasma. Verapamil was used as internal standard. The samples were subjected to a dichloromethane liquid-liquid extraction after ion pairing of the positively charged ammonium compound with iodide prior to LC-MS. Optimized conditions involved separation on a Symmetry Shield RP-18 column (50 x 2.1 mm, 3.5 microm) using a 15-min gradient from 10 to 90% acetonitrile in water containing 0.1% trifluoroacetic acid at 250 microl/min. Linear detector responses for standards were observed from 25 to 2,000 ng/ml. The extraction recovery averaged 59% for rocuronium and 83% for the internal standard. The limit of quantification (LOQ), using 500 microl of plasma, was 25 ng/ml. Precision ranged from 1.3 to 19% (LOQ), and accuracy was between 92 and 112%. In plasma samples, at 20 and 4 degrees C, rocuronium was stable at physiological pH for 4 h; frozen at -30 degrees C it was stable for at least 75 days. The method was found suitable for the analysis of samples collected during pharmacokinetic investigations in humans.

  3. Direct separation of boron from Na- and Ca-rich matrices by sublimation for stable isotope measurement by MC-ICP-MS.

    PubMed

    Wang, Bo-Shian; You, Chen-Feng; Huang, Kuo-Fang; Wu, Shein-Fu; Aggarwal, Suresh Kumar; Chung, Chuan-Hsiung; Lin, Pei-Ying

    2010-09-15

    An improved technique for precise and accurate determination of boron isotopic composition in Na-rich natural waters (groundwater, seawater) and marine biogenic carbonates was developed. This study used a 'micro-sublimation' technique to separate B from natural sample matrices in place of the conventional ion-exchange extraction. By adjusting analyte to appropriate pH, quantitative recovery of boron can be achieved (>98%) and the B procedural blank is limited to <8 pg. An additional mass bias effect in MC-ICP-MS was observed which could not be improved via the standard-sample-standard bracketing or the 'pseudo internal' normalization by Li. Therefore a standard other than NBS SRM 951 was used to monitor plasma condition in order to maintain analytical accuracy. An isotope cross-calibration with results from TIMS shows that the space-charge mass bias on MC-ICP-MS can be successfully corrected using off-line mathematical manipulation. Several reference materials, including the seawater IAPSO and two groundwater standards IAEA-B-2 and IAEA-B-3, were used to validate this approach. We found that the delta(11)B of the reference coral JCp-1 was 24.22+/-0.28 per thousand, corresponding to seawater pH based on the coral delta(11)B-pH function. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  4. 40 CFR 63.686 - Standards: Oil-water and organic-water separators.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 10 2011-07-01 2011-07-01 false Standards: Oil-water and organic-water... Operations § 63.686 Standards: Oil-water and organic-water separators. (a) The provisions of this section apply to the control of air emissions from oil-water separators and organic-water separators for which...

  5. 40 CFR 63.686 - Standards: Oil-water and organic-water separators.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 10 2010-07-01 2010-07-01 false Standards: Oil-water and organic-water... Operations § 63.686 Standards: Oil-water and organic-water separators. (a) The provisions of this section apply to the control of air emissions from oil-water separators and organic-water separators for which...

  6. 40 CFR 63.686 - Standards: Oil-water and organic-water separators.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 11 2014-07-01 2014-07-01 false Standards: Oil-water and organic-water... Operations § 63.686 Standards: Oil-water and organic-water separators. (a) The provisions of this section apply to the control of air emissions from oil-water separators and organic-water separators for which...

  7. 40 CFR 63.686 - Standards: Oil-water and organic-water separators.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 11 2012-07-01 2012-07-01 false Standards: Oil-water and organic-water... Operations § 63.686 Standards: Oil-water and organic-water separators. (a) The provisions of this section apply to the control of air emissions from oil-water separators and organic-water separators for which...

  8. 40 CFR 63.686 - Standards: Oil-water and organic-water separators.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 11 2013-07-01 2013-07-01 false Standards: Oil-water and organic-water... Operations § 63.686 Standards: Oil-water and organic-water separators. (a) The provisions of this section apply to the control of air emissions from oil-water separators and organic-water separators for which...

  9. Reliability of internal oblique elbow radiographs for measuring displacement of medial epicondyle humerus fractures: a cadaveric study.

    PubMed

    Gottschalk, Hilton P; Bastrom, Tracey P; Edmonds, Eric W

    2013-01-01

    Standard elbow radiographs (AP and lateral views) are not accurate enough to measure true displacement of medial epicondyle fractures of the humerus. The amount of perceived displacement has been used to determine treatment options. This study assesses the utility of internal oblique radiographs for measurement of true displacement in these fractures. A medial epicondyle fracture was created in a cadaveric specimen. Displacement of the fragment (mm) was set at 5, 10, and 15 in line with the vector of the flexor pronator mass. The fragment was sutured temporarily in place. Radiographs were obtained at 0 (AP), 15, 30, 45, 60, 75, and 90 degrees (lateral) of internal rotation, with the elbow in set positions of flexion. This was done with and without radio-opaque markers placed on the fragment and fracture bed. The 45 and 60 degrees internal oblique radiographs were then presented to 5 separate reviewers (of different levels of training) to evaluate intraobserver and interobserver agreement. Change in elbow position did not affect the perceived displacement (P=0.82) with excellent intraobserver reliability (intraclass correlation coefficient range, 0.979 to 0.988) and interobserver agreement of 0.953. The intraclass correlation coefficient for intraobserver reliability on 45 degrees internal oblique films for all groups ranged from 0.985 to 0.998, with interobserver agreement of 0.953. For predicting displacement, the observers were 60% accurate in predicting the true displacement on the 45 degrees internal oblique films and only 35% accurate using the 60 degrees internal oblique view. Standardizing to a 45 degrees internal oblique radiograph of the elbow (regardless of elbow flexion) can augment the treating surgeon's ability to determine true displacement. At this degree of rotation, the measured number can be multiplied by 1.4 to better estimate displacement. The addition of a 45 degrees internal oblique radiograph in medial humeral epicondyle fractures has good intraobserver and interobserver reliability to more accurately estimate the true displacement of these fractures. Diagnostic study, Level II (Development of diagnostic study with universally applied reference "gold" standard).

  10. 26 CFR 1.414(r)-8 - Separate application of section 410(b).

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 26 Internal Revenue 5 2012-04-01 2011-04-01 true Separate application of section 410(b). 1.414(r)-8 Section 1.414(r)-8 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-8 Separate application of section 410(b). (a) General rule. If an employer is treated as...

  11. 26 CFR 1.414(r)-8 - Separate application of section 410(b).

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 26 Internal Revenue 5 2014-04-01 2014-04-01 false Separate application of section 410(b). 1.414(r)-8 Section 1.414(r)-8 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-8 Separate application of section 410(b). (a) General rule. If an employer is treated as...

  12. 26 CFR 1.414(r)-10 - Separate application of section 129(d)(8). [Reserved

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 26 Internal Revenue 5 2013-04-01 2013-04-01 false Separate application of section 129(d)(8). [Reserved] 1.414(r)-10 Section 1.414(r)-10 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE... Plans, Etc. § 1.414(r)-10 Separate application of section 129(d)(8). [Reserved] ...

  13. 26 CFR 1.414(r)-10 - Separate application of section 129(d)(8). [Reserved

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 26 Internal Revenue 5 2012-04-01 2011-04-01 true Separate application of section 129(d)(8). [Reserved] 1.414(r)-10 Section 1.414(r)-10 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE... Plans, Etc. § 1.414(r)-10 Separate application of section 129(d)(8). [Reserved] ...

  14. 26 CFR 1.414(r)-10 - Separate application of section 129(d)(8). [Reserved

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 5 2011-04-01 2011-04-01 false Separate application of section 129(d)(8). [Reserved] 1.414(r)-10 Section 1.414(r)-10 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE... Plans, Etc. § 1.414(r)-10 Separate application of section 129(d)(8). [Reserved] ...

  15. 26 CFR 1.414(r)-8 - Separate application of section 410(b).

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 5 2011-04-01 2011-04-01 false Separate application of section 410(b). 1.414(r)-8 Section 1.414(r)-8 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-8 Separate application of section 410(b). (a) General rule. If an employer is treated as...

  16. 26 CFR 1.414(r)-10 - Separate application of section 129(d)(8). [Reserved

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 26 Internal Revenue 5 2014-04-01 2014-04-01 false Separate application of section 129(d)(8). [Reserved] 1.414(r)-10 Section 1.414(r)-10 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE... Plans, Etc. § 1.414(r)-10 Separate application of section 129(d)(8). [Reserved] ...

  17. 26 CFR 1.414(r)-8 - Separate application of section 410(b).

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 26 Internal Revenue 5 2013-04-01 2013-04-01 false Separate application of section 410(b). 1.414(r)-8 Section 1.414(r)-8 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-8 Separate application of section 410(b). (a) General rule. If an employer is treated as...

  18. ["Epistemic Negotiations" and the Pluralism of the Radiation Protection Regime: The Determination of Radiation Protection Standards for the General Population in the Early Years After World War II].

    PubMed

    Higuchi, Toshihiro

    2015-10-01

    Radiation protection standards for the general population have constituted one of the most controversial subjects in the history of atomic energy uses. This paper reexamines the process in which the first such standards evolved in the early postwar period. While the existing literature has emphasized a "collusion" between the standard-setters and users, the paper seeks to examine the horizontal relationship among the standard-setters. It first examines a series of expert consultations between the United States and the United Kingdom. Representing a different configuration of power and interest, the two failed to agree on the assessment of genetic damage and cancer induction whose occurrence might have no threshold and therefore be dependent on the population size. This stalemate prevented the International Commission on Radiological Protection (ICRP), established in 1950, from formulating separate guidelines for the general public. Situations radically changed when the Bikini incident in 1954 led to the creation of more scientific panels. One such panel under the U.S. Academy of Sciences enabled the geneticists to bridge their internal divide, unanimously naming 100 mSv as the genetically permissible dose for the general population. Not to be outdone, ICRP publicized its own guidelines for the same purpose. The case examined in this paper shows that the standard-setting process is best understood as a series of "epistemic negotiations" among and within the standard-setters, whose agendas were determined from the outset but whose outcomes were not.

  19. The Rubidium-Crystal Oscillator Hybrid Development Program

    NASA Technical Reports Server (NTRS)

    Vig, J. R.; Rosati, V. J.

    1984-01-01

    The rubidium-crystal oscillator hybrid (RbXO) will make precise time available to systems that lack the power required by atomic frequency standards. The RbXO consists of two subassemblies in separate enclosures. One contains a small rubidium frequency standard (RFS) without its internal oven-controlled crystal oscillator (OCXO), plus interface circuits. The second contains a low-power OCXO, and additional interface circuits. The OCXO is on continuously. Periodically, e.g., once a week, the user system applies power to the RFS. After the few necessary for the warmup of the RFS, the interface circuits adjust the frequency of the OCXO to the RFS reference, then shut off the RFS. The OCXO enclosure is separable from the RFS enclosure so that manpacks will be able to operate with minimum size, weight, and power consumption, while having the accuracy of the RFS for the duration of a mission. A prototype RbXO's RFS has operated successfully for 4200 on-off cycles. Parallel efforts on a Phase 2 RbXO development are in progress. Two sources for the RbXO are scheduled to be available during 1986.

  20. DIGE Analysis of Human Tissues.

    PubMed

    Gelfi, Cecilia; Capitanio, Daniele

    2018-01-01

    Two-dimensional difference gel electrophoresis (2-D DIGE) is an advanced and elegant gel electrophoretic analytical tool for comparative protein assessment. It is based on two-dimensional gel electrophoresis (2-DE) separation of fluorescently labeled protein extracts. The tagging procedures are designed to not interfere with the chemical properties of proteins with respect to their pI and electrophoretic mobility, once a proper labeling protocol is followed. The two-dye or three-dye systems can be adopted and their choice depends on specific applications. Furthermore, the use of an internal pooled standard makes 2-D DIGE a highly accurate quantitative method enabling multiple protein samples to be separated on the same two-dimensional gel. The image matching and cross-gel statistical analysis generates robust quantitative results making data validation by independent technologies successful.

  1. 26 CFR 1.665(g)-2A - Application of separate share rule.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 8 2011-04-01 2011-04-01 false Application of separate share rule. 1.665(g)-2A Section 1.665(g)-2A Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED... Taxable Years Beginning on Or After January 1, 1969 § 1.665(g)-2A Application of separate share rule. (a...

  2. 26 CFR 1.665(g)-2A - Application of separate share rule.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 26 Internal Revenue 8 2013-04-01 2013-04-01 false Application of separate share rule. 1.665(g)-2A Section 1.665(g)-2A Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED... Taxable Years Beginning on Or After January 1, 1969 § 1.665(g)-2A Application of separate share rule. (a...

  3. 26 CFR 1.665(g)-2A - Application of separate share rule.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 26 Internal Revenue 8 2012-04-01 2012-04-01 false Application of separate share rule. 1.665(g)-2A Section 1.665(g)-2A Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED... Taxable Years Beginning on Or After January 1, 1969 § 1.665(g)-2A Application of separate share rule. (a...

  4. 26 CFR 1.665(g)-2A - Application of separate share rule.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 8 2010-04-01 2010-04-01 false Application of separate share rule. 1.665(g)-2A Section 1.665(g)-2A Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED... Years Beginning on Or After January 1, 1969 § 1.665(g)-2A Application of separate share rule. (a) In...

  5. 26 CFR 1.665(g)-2A - Application of separate share rule.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 26 Internal Revenue 8 2014-04-01 2014-04-01 false Application of separate share rule. 1.665(g)-2A Section 1.665(g)-2A Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED... Taxable Years Beginning on Or After January 1, 1969 § 1.665(g)-2A Application of separate share rule. (a...

  6. Establishment of the 2nd Korean national biological reference standard for blood coagulation factor VIII:C concentrate.

    PubMed

    Lee, Naery; Seo, Ji Suk; Kim, Jae Ok; Ban, Sang Ja

    2017-05-01

    Since the 1st Korean national biological reference standard for factor (F)VIII concentrate, established in 2001, has shown declining potency, we conducted this study to replace this standard with a 2nd Korean national biological reference standard for blood coagulation FVIII concentrate. The candidate materials for the 2nd standard were prepared in 8000 vials with 10 IU/ml of target potency, according to the approved manufacturing process of blood coagulation Factor VIII:C Monoclonal Antibody-purified, Freeze-dried Human Blood Coagulation Factor VIII:C. Potency was evaluated by one-stage clotting and chromogenic methods and the stability was confirmed to meet the specifications during a period of 73 months. Since the potencies obtained by the two methods differed significantly (P < 0.015), the values were determined separately according to the geometric means (8.9 and 7.4 IU/vial, respectively). The geometric coefficients of interlaboratory variability were 3.4% and 7.6% by the one-stage clotting and chromogenic assays, respectively. Copyright © 2017 International Alliance for Biological Standardization. Published by Elsevier Ltd. All rights reserved.

  7. Adolescent-Peer Relationships, Separation and Detachment from Parents, and Internalizing and Externalizing Behaviors: Linkages and Interactions

    PubMed Central

    Jager, Justin; Yuen, Cynthia X.; Putnick, Diane L.; Hendricks, Charlene; Bornstein, Marc H.

    2018-01-01

    Most research exploring the interplay between context and adolescent separation and detachment has focused on the family; in contrast, this investigation directs its attention outside of the family to peers. Utilizing a latent variable approach for modeling interactions and incorporating reports of behavioral adjustment from 14-year-old adolescents (N = 190) and their mothers, we examine how separation and detachment relate to adolescent peer relationships, and whether peer relationships moderate how separation and detachment relate to adolescent internalizing and externalizing behaviors. Positive peer relationships were both associated with lower detachment and sharply attenuated relations between detachment and higher adolescent internalizing and externalizing. Separation from parents was unrelated to peer relationships, and regardless of whether peer relationships were positive, separation was not related to adolescent internalizing and externalizing. We integrate these findings with those from family-focused investigations and discuss their substantive and clinical implications. PMID:29527086

  8. 76 FR 16240 - Mandatory Reliability Standards for Interconnection Reliability Operating Limits

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-03-23

    ... Standards. The Reliability Standards were designed to prevent instability, uncontrolled separation, or... designed to prevent instability, uncontrolled separation, or cascading outages that adversely impact the... instability, uncontrolled separation, or cascading outages. See NERC Glossary, available at http://www.nerc...

  9. 26 CFR 1.614-4 - Treatment under the Internal Revenue Code of 1939 with respect to separate operating mineral...

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 7 2010-04-01 2010-04-01 true Treatment under the Internal Revenue Code of 1939..., in the case of oil and gas wells. 1.614-4 Section 1.614-4 Internal Revenue INTERNAL REVENUE SERVICE....614-4 Treatment under the Internal Revenue Code of 1939 with respect to separate operating mineral...

  10. Enantiomeric separation and quantification of R/S-amphetamine in urine by ultra-high performance supercritical fluid chromatography tandem mass spectrometry.

    PubMed

    Hegstad, S; Havnen, H; Helland, A; Spigset, O; Frost, J

    2018-03-01

    To distinguish between legal and illegal consumption of amphetamine reliable analytical methods for chiral separation of the R- and S-enantiomers of amphetamine in biological specimens are required. In this regard, supercritical fluid chromatography (SFC) has several potential advantages over liquid chromatography, including rapid separation of enantiomers due to low viscosity and high diffusivity of supercritical carbon dioxide, the main component in the SFC mobile phase. A method for enantiomeric separation and quantification of R- and S-amphetamine in urine was developed and validated using ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS). Sample preparation prior to UHPSFC-MS/MS analysis was a semi-automatic solid phase extraction method. The UHPSFC-MS/MS method used a Chiralpak AD-3 column with a mobile phase consisting of CO 2 and 0.2% cyclohexylamine in 2-propanol. The injection volume was 2 μL and run-time was 6 min. MS/MS detection was performed with positive electrospray ionization and two multiple reaction monitoring transitions (m/z 136.1 > 119.0 and m/z 136.1 > 91.0). The calibration range was 50-10,000 ng/mL for each enantiomer. The between-assay relative standard deviations were in the range of 3.7-7.6%. Recovery was 92-93% and matrix effects ranged from 100 to 104% corrected with internal standard. After development and validation, the method has been successfully implemented in routine use at our laboratory for both separation and quantification of R/S-amphetamine, and has proved to be a reliable and useful tool for distinguishing intake of R- and S-amphetamine in authentic patient samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  11. Global perspectives on ensuring the safety of pharmaceutical products in the distribution process
.

    PubMed

    Jeong, Sohyun; Ji, Eunhee

    2018-01-01

    The distribution of counterfeit or falsified drugs is increasing worldwide. This can contribute to the high burden of disease and cost to society and is of global concern with the worldwide circulation of pharmaceuticals. The preparation and implementation of good distribution practice should be one of the most important aspects of ensuring safe drug circulation and administration. This research aimed to compare and analyze good distribution practice guidelines from advanced countries and international organizations, and to evaluate the status of the current good distribution practice guidelines in the world. Advanced pharmaceutical countries and international organizations, such as the World Health Organization, European Union, Pharmaceutical Inspection Co-operation Scheme, United States of America, Canada, and Australia, which have stable good distribution practice guidelines and public confidence, were included in the analysis. The World Health Organization and European Union guidelines are models for standardized good distribution practice for nations worldwide. The United States of America has a combination of four different series of distribution practices which have a unique structure and detailed content compared to those of other countries. The Canadian guidelines focus on temperature control during storage and transportation. The Australian guidelines apply to both classes of medicinal products and medical devices and need separate standardization. Transparent information about the Internet chain, international cooperation regarding counterfeiting, a high-standard qualification of sellers and customers, and technology to track and trace the whole life cycle of drugs should be the main focus of future good distribution practice guidelines worldwide.
.

  12. Validation of neural spike sorting algorithms without ground-truth information.

    PubMed

    Barnett, Alex H; Magland, Jeremy F; Greengard, Leslie F

    2016-05-01

    The throughput of electrophysiological recording is growing rapidly, allowing thousands of simultaneous channels, and there is a growing variety of spike sorting algorithms designed to extract neural firing events from such data. This creates an urgent need for standardized, automatic evaluation of the quality of neural units output by such algorithms. We introduce a suite of validation metrics that assess the credibility of a given automatic spike sorting algorithm applied to a given dataset. By rerunning the spike sorter two or more times, the metrics measure stability under various perturbations consistent with variations in the data itself, making no assumptions about the internal workings of the algorithm, and minimal assumptions about the noise. We illustrate the new metrics on standard sorting algorithms applied to both in vivo and ex vivo recordings, including a time series with overlapping spikes. We compare the metrics to existing quality measures, and to ground-truth accuracy in simulated time series. We provide a software implementation. Metrics have until now relied on ground-truth, simulated data, internal algorithm variables (e.g. cluster separation), or refractory violations. By contrast, by standardizing the interface, our metrics assess the reliability of any automatic algorithm without reference to internal variables (e.g. feature space) or physiological criteria. Stability is a prerequisite for reproducibility of results. Such metrics could reduce the significant human labor currently spent on validation, and should form an essential part of large-scale automated spike sorting and systematic benchmarking of algorithms. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. The application of standard definitions of sound to the fields of underwater acoustics and acoustical oceanography

    NASA Astrophysics Data System (ADS)

    Carey, William M.

    2004-05-01

    Recent societal concerns have focused attention on the use of sound as a probe to investigate the oceans and its use in naval sonar applications. The concern is the impact the use of sound may have on marine mammals and fishes. The focus has changed the fields of acoustical oceanography (AO) and underwater acoustics (UW) because of the requirement to communicate between disciplines. Multiple National Research Council publications, Dept. of Navy reports, and several monographs have been written on this subject, and each reveals the importance as well as the misapplication of ASA standards. The ANSI-ASA standards are comprehensive, however not widely applied. The clear definition of standards and recommendations of their use is needed for both scientists and government agencies. Traditionally the U.S. Navy has been responsible for UW standards and calibration; the ANSI-ASA standards have been essential. However, recent changes in the Navy and its laboratory structure may necessitate a more formal recognition of ANSI-ASA standards and perhaps incorporation of UW-AO in the Bureau of Standards. A separate standard for acoustical terminology, reference levels, and notation used in the UW-AO is required. Since the problem is global, a standard should be compatible and cross referenced with the International Standard (CEI/IEC 27-3).

  14. Analysis of amino acids by HPLC/electrospray negative ion tandem mass spectrometry using 9-fluorenylmethoxycarbonyl chloride (Fmoc-Cl) derivatization.

    PubMed

    Ziegler, Jörg; Abel, Steffen

    2014-12-01

    A new method for the determination of amino acids is presented. It combines established methods for the derivatization of primary and secondary amino groups with 9-fluorenylmethoxycarbonyl chloride (Fmoc-Cl) with the subsequent amino acid specific detection of the derivatives by LC-ESI-MS/MS using multiple reaction monitoring (MRM). The derivatization proceeds within 5 min, and the resulting amino acid derivatives can be rapidly purified from matrix by solid-phase extraction (SPE) on HR-X resin and separated by reversed-phase HPLC. The Fmoc derivatives yield several amino acid specific fragment ions which opened the possibility to select amino acid specific MRM transitions. The method was applied to all 20 proteinogenic amino acids, and the quantification was performed using L-norvaline as standard. A limit of detection as low as 1 fmol/µl with a linear range of up to 125 pmol/µl could be obtained. Intraday and interday precisions were lower than 10 % relative standard deviations for most of the amino acids. Quantification using L-norvaline as internal standard gave very similar results compared to the quantification using deuterated amino acid as internal standards. Using this protocol, it was possible to record the amino acid profiles of only a single root from Arabidopsis thaliana seedlings and to compare it with the amino acid profiles of 20 dissected root meristems (200 μm).

  15. Improving efficiency and reducing administrative burden through electronic communication.

    PubMed

    Cook, Katlyn E; Ludens, Gail M; Ghosh, Amit K; Mundell, William C; Fleming, Kevin C; Majka, Andrew J

    2013-01-01

    The InBox messaging system is an internal, electronic program used at Mayo Clinic, Rochester, MN, to facilitate the sending, receiving, and answering of patient-specific messages and alerts. A standardized InBox was implemented in the Division of General Internal Medicine to decrease the time physicians, physician assistants, and nurse practitioners (clinicians) spend on administrative tasks and to increase efficiency. Clinicians completed surveys and a preintervention InBox pilot test to determine inefficiencies related to administrative burdens and defects (message entry errors). Results were analyzed using Pareto diagrams, value stream mapping, and root cause analysis to prioritize administrative-burden inefficiencies to develop a new, standardized InBox. Clinicians and allied health staff were the target of this intervention and received standardized InBox training followed by a postintervention pilot test for clinicians. Sixteen of 28 individuals (57%) completed the preintervention survey. Twenty-eight clinicians participated in 2 separate 8-day pilot tests (before and after intervention) for the standardized InBox. The number of InBox defects was substantially reduced from 37 (Pilot 1) to 7 (Pilot 2). Frequent InBox defects decreased from 25% to 10%. More than half of clinicians believed the standardized InBox positively affected their work, and 100% of clinicians reported no negative affect on their work. This project demonstrated the successful implementation of the standardized InBox messaging system. Initial assessments show substantial reduction of InBox entry defects and administrative tasks completed by clinicians. The findings of this project suggest increased clinician and allied health staff efficiency, satisfaction, improved clinician work-life balance, and decreased clinician burden caused by administrative tasks.

  16. New conducted electrical weapons: Electrical safety relative to relevant standards.

    PubMed

    Panescu, Dorin; Nerheim, Max; Kroll, Mark W; Brave, Michael A

    2017-07-01

    We have previously published about TASER ® conducted electrical weapons (CEW) compliance with international standards. CEWs deliver electrical pulses that can inhibit a person's neuromuscular control or temporarily incapacitate. An eXperimental Rotating-Field (XRF) waveform CEW and the X2 CEW are new 2-shot electrical weapon models designed to target a precise amount of delivered charge per pulse. They both can deploy 1 or 2 dart pairs, delivered by 2 separate cartridges. Additionally, the XRF controls delivery of incapacitating pulses over 4 field vectors, in a rotating sequence. As in our previous study, we were motivated by the need to understand the cardiac safety profile of these new CEWs. The goal of this paper is to analyze the nominal electrical outputs of TASER XRF and X2 CEWs in reference to provisions of all relevant international standards that specify safety requirements for electrical medical devices and electrical fences. Although these standards do not specifically mention CEWs, they are the closest electrical safety standards and hence give very relevant guidance. The outputs of several TASER XRF and X2 CEWs were measured under normal operating conditions. The measurements were compared against manufacturer specifications. CEWs electrical output parameters were reviewed against relevant safety requirements of UL 69, IEC 60335-2-76 Ed 2.1, IEC 60479-1, IEC 60479-2, AS/NZS 60479.1, AS/NZS 60479.2, IEC 60601-1 and BS EN 60601-1. Our study confirmed that the nominal electrical outputs of TASER XRF and X2 CEWs lie within safety bounds specified by relevant standards.

  17. Determination of benzylpenicillin in pharmaceuticals by capillary zone electrophoresis

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

    Hoyt, A.M. Jr.; Sepaniak, M.J.

    A rapid and direct method is described for the determination of benzylpenicillin (penicillin G) in pharmaceutical preparations. The method involves very little sample preparation and total analysis time for duplicate results is less 30 minutes per sample. The method takes advantage of the speed and separating power of capillary zone electrophoresis (CZE). Detection of penicillin is by absorption at 228 nm. An internal standard is employed to reduce sample injection error. The method was applied successfully to both tablets and injectable preparations. 14 refs., 5 figs., 3 tabs.

  18. An Operational Wake Vortex Sensor Using Pulsed Coherent Lidar

    NASA Technical Reports Server (NTRS)

    Barker, Ben C., Jr.; Koch, Grady J.; Nguyen, D. Chi

    1998-01-01

    NASA and FAA initiated a program in 1994 to develop methods of setting spacings for landing aircraft by incorporating information on the real-time behavior of aircraft wake vortices. The current wake separation standards were developed in the 1970's when there was relatively light airport traffic and a logical break point by which to categorize aircraft. Today's continuum of aircraft sizes and increased airport packing densities have created a need for re-evaluation of wake separation standards. The goals of this effort are to ensure that separation standards are adequate for safety and to reduce aircraft spacing for higher airport capacity. Of particular interest are the different requirements for landing under visual flight conditions and instrument flight conditions. Over the years, greater spacings have been established for instrument flight than are allowed for visual flight conditions. Preliminary studies indicate that the airline industry would save considerable money and incur fewer passenger delays if a dynamic spacing system could reduce separations at major hubs during inclement weather to the levels routinely achieved under visual flight conditions. The sensor described herein may become part of this dynamic spacing system known as the "Aircraft VOrtex Spacing System" (AVOSS) that will interface with a future air traffic control system. AVOSS will use vortex behavioral models and short-term weather prediction models in order to predict vortex behavior sufficiently into the future to allow dynamic separation standards to be generated. The wake vortex sensor will periodically provide data to validate AVOSS predictions. Feasibility of measuring wake vortices using a lidar was first demonstrated using a continuous wave (CW) system from NASA Marshall Space Flight Sensor and tested at the Volpe National Transportation Systems Center's wake vortex test site at JFK International Airport. Other applications of CW lidar for wake vortex measurement have been made more recently, including a system developed by the MIT Lincoln Laboratory. This lidar has been used for detailed measurements of wake vortex velocities in support of wake vortex model validation. The first measurements of wake vortices using a pulsed, lidar were made by Coherent Technologies, Inc. (CTI) using a 2 micron solid-state, flashlamp-pumped system operating at 5 Hz. This system was first deployed at Denver's Stapleton Airport. Pulsed lidar has been selected as the baseline technology for an operational sensor due to its longer range capability.

  19. Halogenated peptides as internal standards (H-PINS): introduction of an MS-based internal standard set for liquid chromatography-mass spectrometry.

    PubMed

    Mirzaei, Hamid; Brusniak, Mi-Youn; Mueller, Lukas N; Letarte, Simon; Watts, Julian D; Aebersold, Ruedi

    2009-08-01

    As the application for quantitative proteomics in the life sciences has grown in recent years, so has the need for more robust and generally applicable methods for quality control and calibration. The reliability of quantitative proteomics is tightly linked to the reproducibility and stability of the analytical platforms, which are typically multicomponent (e.g. sample preparation, multistep separations, and mass spectrometry) with individual components contributing unequally to the overall system reproducibility. Variations in quantitative accuracy are thus inevitable, and quality control and calibration become essential for the assessment of the quality of the analyses themselves. Toward this end, the use of internal standards cannot only assist in the detection and removal of outlier data acquired by an irreproducible system (quality control) but can also be used for detection of changes in instruments for their subsequent performance and calibration. Here we introduce a set of halogenated peptides as internal standards. The peptides are custom designed to have properties suitable for various quality control assessments, data calibration, and normalization processes. The unique isotope distribution of halogenated peptides makes their mass spectral detection easy and unambiguous when spiked into complex peptide mixtures. In addition, they were designed to elute sequentially over an entire aqueous to organic LC gradient and to have m/z values within the commonly scanned mass range (300-1800 Da). In a series of experiments in which these peptides were spiked into an enriched N-glycosite peptide fraction (i.e. from formerly N-glycosylated intact proteins in their deglycosylated form) isolated from human plasma, we show the utility and performance of these halogenated peptides for sample preparation and LC injection quality control as well as for retention time and mass calibration. Further use of the peptides for signal intensity normalization and retention time synchronization for selected reaction monitoring experiments is also demonstrated.

  20. Development of visual peak selection system based on multi-ISs normalization algorithm to apply to methamphetamine impurity profiling.

    PubMed

    Lee, Hun Joo; Han, Eunyoung; Lee, Jaesin; Chung, Heesun; Min, Sung-Gi

    2016-11-01

    The aim of this study is to improve resolution of impurity peaks using a newly devised normalization algorithm for multi-internal standards (ISs) and to describe a visual peak selection system (VPSS) for efficient support of impurity profiling. Drug trafficking routes, location of manufacture, or synthetic route can be identified from impurities in seized drugs. In the analysis of impurities, different chromatogram profiles are obtained from gas chromatography and used to examine similarities between drug samples. The data processing method using relative retention time (RRT) calculated by a single internal standard is not preferred when many internal standards are used and many chromatographic peaks present because of the risk of overlapping between peaks and difficulty in classifying impurities. In this study, impurities in methamphetamine (MA) were extracted by liquid-liquid extraction (LLE) method using ethylacetate containing 4 internal standards and analyzed by gas chromatography-flame ionization detection (GC-FID). The newly developed VPSS consists of an input module, a conversion module, and a detection module. The input module imports chromatograms collected from GC and performs preprocessing, which is converted with a normalization algorithm in the conversion module, and finally the detection module detects the impurities in MA samples using a visualized zoning user interface. The normalization algorithm in the conversion module was used to convert the raw data from GC-FID. The VPSS with the built-in normalization algorithm can effectively detect different impurities in samples even in complex matrices and has high resolution keeping the time sequence of chromatographic peaks the same as that of the RRT method. The system can widen a full range of chromatograms so that the peaks of impurities were better aligned for easy separation and classification. The resolution, accuracy, and speed of impurity profiling showed remarkable improvement. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

  1. Simultaneous determination of atenolol, chlorthalidone and amiloride in pharmaceutical preparations by capillary zone electrophoresis with ultraviolet detection.

    PubMed

    Al Azzam, Khaldun M; Saad, Bahruddin; Aboul-Enein, Hassan Y

    2010-09-01

    Capillary zone electrophoresis methods for the simultaneous determination of the beta-blocker drugs, atenolol, chlorthalidone and amiloride, in pharmaceutical formulations have been developed. The influences of several factors (buffer pH, concentration, applied voltage, capillary temperature and injection time) were studied. Using phenobarbital as internal standard, the analytes were all separated in less than 4 min. The separation was carried out in normal polarity mode at 25 degrees C, 25 kV and using hydrodynamic injection (10 s). The separation was effected in an uncoated fused-silica capillary (75 mum i.d. x 52 cm) and a background electrolyte of 25 mm H(3)PO(4) adjusted with 1 m NaOH solution (pH 9.0) and detection at 198 nm. The method was validated with respect to linearity, limit of detection and quantification, accuracy, precision and selectivity. Calibration curves were linear over the range 1-250 microg/mL for atenolol and chlorthalidone and from 2.5-250 microg/mL for amiloride. The relative standard deviations of intra- and inter-day migration times and corrected peak areas were less than 6.0%. The method showed good precision and accuracy and was successfully applied to the simultaneous determination of atenolol, chlorthalidone and amiloride in various pharmaceutical tablets formulations. 2010 John Wiley & Sons, Ltd.

  2. Application of ultra-high performance supercritical fluid chromatography for the determination of carotenoids in dietary supplements.

    PubMed

    Li, Bing; Zhao, Haiyan; Liu, Jing; Liu, Wei; Fan, Sai; Wu, Guohua; Zhao, Rong

    2015-12-18

    A quick and simple ultra-high performance supercritical fluid chromatography-photodiode array detector method was developed and validated for the simultaneous determination of 9 carotenoids in dietary supplements. The influences of stationary phase, co-solvent, pressure, temperature and flow rate on the separation of carotenoids were evaluated. The separation of the carotenoids was carried out using an Acquity UPC(2) HSS C18 SB column (150mm×3.0mm, 1.8μm) by gradient elution with carbon dioxide and a 1:2 (v:v) methanol/ethanol mixture. The column temperature was set to 35°C and the backpressure was 15.2MPa. Under these conditions, 9 carotenoids and the internal standard, β-apo-8'-carotenal, were successfully separated within 10min. The correlation coefficients (R(2)) of the calibration curves were all above 0.997, the limits of detection for the 9 carotenoids were in the range of 0.33-1.08μg/mL, and the limits of quantification were in the range of 1.09-3.58μg/mL. The mean recoveries were from 93.4% to 109.5% at different spiking levels, and the relative standard deviations were between 0.8% and 6.0%. This method was successfully applied to the determination of 9 carotenoids in commercial dietary supplements. Copyright © 2015 Elsevier B.V. All rights reserved.

  3. Standardized training in nurse model travel clinics.

    PubMed

    Sofarelli, Theresa A; Ricks, Jane H; Anand, Rahul; Hale, Devon C

    2011-01-01

    International travel plays a significant role in the emergence and redistribution of major human diseases. The importance of travel medicine clinics for preventing morbidity and mortality has been increasingly appreciated, although few studies have thus far examined the management and staff training strategies that result in successful travel-clinic operations. Here, we describe an example of travel-clinic operation and management coordinated through the University of Utah School of Medicine, Division of Infectious Diseases. This program, which involves eight separate clinics distributed statewide, functions both to provide patient consult and care services, as well as medical provider training and continuing medical education (CME). Initial training, the use of standardized forms and protocols, routine chart reviews and monthly continuing education meetings are the distinguishing attributes of this program. An Infectious Disease team consisting of one medical doctor (MD) and a physician assistant (PA) act as consultants to travel nurses who comprise the majority of clinic staff. Eight clinics distributed throughout the state of Utah serve approximately 6,000 travelers a year. Pre-travel medical services are provided by 11 nurses, including 10 registered nurses (RNs) and 1 licensed practical nurse (LPN). This trained nursing staff receives continuing travel medical education and participate in the training of new providers. All nurses have completed a full training program and 7 of the 11 (64%) of clinic nursing staff serve more than 10 patients a week. Quality assurance measures show that approximately 0.5% of charts reviewed contain a vaccine or prescription error which require patient notification for correction. Using an initial training program, standardized patient intake forms, vaccine and prescription protocols, preprinted prescriptions, and regular CME, highly trained nurses at travel clinics are able to provide standardized pre-travel care to international travelers originating from Utah. © 2010 International Society of Travel Medicine.

  4. Direct determination of N-methyl-2-pyrrolidone metabolites in urine by HPLC-electrospray ionization-MS/MS using deuterium-labeled compounds as internal standard.

    PubMed

    Suzuki, Yoshihiro; Endo, Yoko; Ogawa, Masanori; Yamamoto, Shinobu; Takeuchi, Akito; Nakagawa, Tomoo; Onda, Nobuhiko

    2009-11-01

    N-methyl-2-pyrrolidone (NMP) has been used in many industries and biological monitoring of NMP exposure is preferred to atmospheric monitoring in occupational health. We developed an analytical method that did not include solid phase extraction (SPE) but utilized deuterium-labeled compounds as internal standard for high-performance liquid chromatography-electrospray ionization-mass spectrometry using a C30 column. Urinary concentrations of NMP and its known metabolites 5-hydoxy-N-methyl-2-pyrrolidone (5-HNMP), N-methyl-succinimide (MSI), and 2-hydroxy-N-methylsuccinimide (2-HMSI) were determined in a single run. The method provided baseline separation of these compounds. Their limits of detection in 10-fold diluted urine were 0.0001, 0.006, 0.008, and 0.03 mg/L, respectively. Linear calibration covered a biological exposure index (BEI) for urinary concentration. The within-run and total precisions (CV, %) were 5.6% and 9.2% for NMP, 3.4% and 4.2% for 5-HNMP, 3.7% and 6.0% for MSI, and 6.5% and 6.9% for 2-HMSI. The method was evaluated using international external quality assessment samples, and urine samples from workers exposed to NMP in an occupational area.

  5. [Determination of ferulic acid absorbed into human serum from oral decoction of rhizoma chuanxiong and pharmacokinetic study of ferulic acid].

    PubMed

    Sun, S; Huang, X; Zhang, L; Ren, P; Chang, Z

    2001-10-01

    To improve the HPLC method for determining ferulic acid(FA) in the human serum and to research FA clinical pharmacokinetics. Serum concentrations of FA were determined by HPLC using methanol-water-acetic acid (40:59.7:0.3, v/v) as the mobile phase and the column packed with ODS (150 mm x 4.6 mm, 5 microns) as a fixed phase and the flow rate was 1.0 ml/min. FA was detected at 320 nm wave length. The internal standard was coumarin. The serum samples were treated by the water-boiling method. Peak of FA in serum was recognized by photodiode-array detection. FA and internal standard were separated completely under the condition described as above. FA was linear in the range of (40.16-8032 ng/ml) (r = 0.9975). The CV was less than 10%, the average recovery was 100.3%, and the limit concentration in serum was 25.1 ng/ml. PK was in accordance with open bicameral model. This method can be applied to clinical pharmacokinetic study of FA.

  6. Gas chromatographic quantitation of underivatized amines in the determination of their octanol-0.1 M sodium hydroxide partition coefficients by the shake-flask method.

    PubMed

    Grunewald, G L; Pleiss, M A; Gatchell, C L; Pazhenchevsky, R; Rafferty, M F

    1984-06-01

    The use of gas chromatography (GC) for the determination of 0.1 M sodium hydroxide-octanol partition coefficients (log P) for a wide variety of ethylamines is demonstrated. The conventional shake-flask procedure (SFP) is utilized, with the addition of an internal reference, which is cleanly separated from the desired solute and solvents on a 10% Apiezon L, 2% potassium hydroxide on 80-100 mesh Chromosorb W AW column. The partitioned solute is extracted from the aqueous phase with chloroform and analyzed by GC. The method provides an accurate and highly reproducible means of determining log P values, as demonstrated by the low relative standard errors. The technique is both rapid and extremely versatile. The use of the internal standard method of analysis introduces consistency, since variables like the exact weight of solute are not necessary (unlike the traditional SFP) and the volume of sample injected is not critical. The technique is readily accessible to microgram quantities of solutes, making it ideal for a wide range of volatile, amine-bearing compounds.

  7. Rapid determination of protopine, allocryptopine, sanguinarine and chelerythrine in fruits of Macleaya cordata by microwave-assisted solvent extraction and HPLC-ESI/MS.

    PubMed

    Luo, Xu-Biao; Chen, Bo; Yao, Shou-Zhuo

    2006-01-01

    An isocratic high-performance liquid chromatographic method coupled with electrospray mass spectrometry was developed to determine protopine, allocryptopine, sanguinarine and chelerythrine in fruits of Macleaya cordata. The sample was extracted with hydrochloric acid aqueous solution using microwave-assisted extraction method. The extracts were separated on a C8 reversed-phase HPLC column with acetonitrile:acetate buffer as mobile phase, and full elution of all analytes was realized isocratically within 10 min. The abundance of pseudomolecule ions was recorded using selected ion recording at m/z 354.4, 370.1, 332.5, 348.5 and 338.5 for protopine, allocryptopine, sanguinarine, chelerythrine and the internal standard, jatrorrhizine, respectively. Internal standard curves were used for the quantification of protopine, allocryptopine, sanguinarine and chelerythrine, which showed a linear range of 0.745-74.5, 0.610-61.0, 0.525-105 and 0.375-75 microg/mL, respectively, with correlation coefficients of 0.9995, 0.9992, 0.9993 and 0.9989, and limits of detection of 3.73, 3.05, 1.60 and 1.11 ng/mL, respectively.

  8. NIST/ISAC standardization study: variability in assignment of intensity values to fluorescence standard beads and in cross calibration of standard beads to hard dyed beads.

    PubMed

    Hoffman, Robert A; Wang, Lili; Bigos, Martin; Nolan, John P

    2012-09-01

    Results from a standardization study cosponsored by the International Society for Advancement of Cytometry (ISAC) and the US National Institute of Standards and Technology (NIST) are reported. The study evaluated the variability of assigning intensity values to fluorophore standard beads by bead manufacturers and the variability of cross calibrating the standard beads to stained polymer beads (hard-dyed beads) using different flow cytometers. Hard dyed beads are generally not spectrally matched to the fluorophores used to stain cells, and spectral response varies among flow cytometers. Thus if hard dyed beads are used as fluorescence calibrators, one expects calibration for specific fluorophores (e.g., FITC or PE) to vary among different instruments. Using standard beads surface-stained with specific fluorophores (FITC, PE, APC, and Pacific Blue™), the study compared the measured intensity of fluorophore standard beads to that of hard dyed beads through cross calibration on 133 different flow cytometers. Using robust CV as a measure of variability, the variation of cross calibrated values was typically 20% or more for a particular hard dyed bead in a specific detection channel. The variation across different instrument models was often greater than the variation within a particular instrument model. As a separate part of the study, NIST and four bead manufacturers used a NIST supplied protocol and calibrated fluorophore solution standards to assign intensity values to the fluorophore beads. Values assigned to the reference beads by different groups varied by orders of magnitude in most cases, reflecting differences in instrumentation used to perform the calibration. The study concluded that the use of any spectrally unmatched hard dyed bead as a general fluorescence calibrator must be verified and characterized for every particular instrument model. Close interaction between bead manufacturers and NIST is recommended to have reliable and uniformly assigned fluorescence standard beads. Copyright © 2012 International Society for Advancement of Cytometry.

  9. Determination of some phenolic compounds in red wine by RP-HPLC: method development and validation.

    PubMed

    Burin, Vívian Maria; Arcari, Stefany Grützmann; Costa, Léa Luzia Freitas; Bordignon-Luiz, Marilde T

    2011-09-01

    A methodology employing reversed-phase high-performance liquid chromatography (RP-HPLC) was developed and validated for simultaneous determination of five phenolic compounds in red wine. The chromatographic separation was carried out in a C(18) column with water acidify with acetic acid (pH 2.6) (solvent A) and 20% solvent A and 80% acetonitrile (solvent B) as the mobile phase. The validation parameters included: selectivity, linearity, range, limits of detection and quantitation, precision and accuracy, using an internal standard. All calibration curves were linear (R(2) > 0.999) within the range, and good precision (RSD < 2.6%) and recovery (80-120%) was obtained for all compounds. This method was applied to quantify phenolics in red wine samples from Santa Catarina State, Brazil, and good separation peaks for phenolic compounds in these wines were observed.

  10. Determination of antibacterial flomoxef in serum by capillary electrophoresis.

    PubMed

    Kitahashi, Toshihiro; Furuta, Itaru

    2003-04-01

    A determination method of flomoxef (FMOX) concentration in serum by capillary electrophoresis is developed. Serum samples are extracted with acetonitrile. After pretreatment, they are separated in a fused-silica capillary tube with a 25 mM borate buffer (pH 10.0) as a running buffer that contains 50mM sodium dodecyl sulfate. The FMOX and acetaminophen (internal standard) are detected by UV absorbance at 200 nm. Linearity (0-200 mg/L) is good, and the minimum limit of detection is 1.0 mg/L (S/N = 3). The relative standard deviations of intra- and interassay variability are 1.60-4.78% and 2.10-3.31%, respectively, and the recovery rate is 84-98%. This method can be used for determination of FMOX concentration in serum.

  11. 26 CFR 1.985-3 - United States dollar approximate separate transactions method.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... transactions method. 1.985-3 Section 1.985-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE... dollar approximate separate transactions method. (a) Scope and effective date—(1) Scope. This section describes the United States dollar (dollar) approximate separate transactions method of accounting (DASTM...

  12. The PANDA Barrel DIRC

    NASA Astrophysics Data System (ADS)

    Schwiening, J.; Ali, A.; Belias, A.; Dzhygadlo, R.; Gerhardt, A.; Götzen, K.; Kalicy, G.; Krebs, M.; Lehmann, D.; Nerling, F.; Patsyuk, M.; Peters, K.; Schepers, G.; Schmitt, L.; Schwarz, C.; Traxler, M.; Böhm, M.; Eyrich, W.; Lehmann, A.; Pfaffinger, M.; Uhlig, F.; Düren, M.; Etzelmüller, E.; Föhl, K.; Hayrapetyan, A.; Kreutzfeld, K.; Merle, O.; Rieke, J.; Schmidt, M.; Wasem, T.; Achenbach, P.; Cardinali, M.; Hoek, M.; Lauth, W.; Schlimme, S.; Sfienti, C.; Thiel, M.

    2018-03-01

    The PANDA experiment at the international accelerator Facility for Antiproton and Ion Research in Europe (FAIR) near GSI, Darmstadt, Germany will address fundamental questions of hadron physics. Excellent Particle Identification (PID) over a large range of solid angles and particle momenta will be essential to meet the objectives of the rich physics program. Charged PID for the barrel region of the PANDA target spectrometer will be provided by a DIRC (Detection of Internally Reflected Cherenkov light) detector. The Barrel DIRC will cover the polar angle range of 22o-140o and cleanly separate charged pions from kaons for momenta between 0.5 GeV/c and 3.5 GeV/c with a separation power of at least 3 standard deviations. The design is based on the successful BABAR DIRC and the SuperB FDIRC R&D with several important improvements to optimize the performance for PANDA, such as a focusing lens system, fast timing, a compact fused silica prism as expansion region, and lifetime-enhanced Microchannel-Plate PMTs for photon detection. This article describes the technical design of the PANDA Barrel DIRC and the result of the design validation using a "vertical slice" prototype in hadronic particle beams at the CERN PS.

  13. Mitigating external and internal cathode fouling using a polymer bonded separator in microbial fuel cells.

    PubMed

    Yang, Wulin; Rossi, Ruggero; Tian, Yushi; Kim, Kyoung-Yeol; Logan, Bruce E

    2018-02-01

    Microbial fuel cell (MFC) cathodes rapidly foul when treating domestic wastewater, substantially reducing power production over time. Here a wipe separator was chemically bonded to an activated carbon air cathode using polyvinylidene fluoride (PVDF) to mitigate cathode fouling and extend cathode performance over time. MFCs with separator-bonded cathodes produced a maximum power density of 190 ± 30 mW m -2 after 2 months of operation using domestic wastewater, which was ∼220% higher than controls (60 ± 50 mW m -2 ) with separators that were not chemically bonded to the cathode. Less biomass (protein) was measured on the bonded separator surface than the non-bonded separator, indicating chemical bonding reduced external bio-fouling. Salt precipitation that contributed to internal fouling was also reduced using separator-bonded cathodes. Overall, the separator-bonded cathodes showed better performance over time by mitigating both external bio-fouling and internal salt fouling. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. 40 CFR 61.347 - Standards: Oil-water separators.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 9 2014-07-01 2014-07-01 false Standards: Oil-water separators. 61.347 Section 61.347 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS National Emission Standard for Benzene Waste Operations § 61.347 Standards:...

  15. Use of vancomycin silica stationary phase in packed capillary electrochromatography. II. Enantiomer separation of venlafaxine and O-desmethylvenlafaxine in human plasma.

    PubMed

    Fanali, S; Rudaz, S; Veuthey, J L; Desiderio, C

    2001-06-01

    A capillary electrochromatography method, using vancomycin chiral stationary phase packed capillary, was optimized for the simultaneous chiral separation of the antidepressant drug venlafaxine and its main active metabolite O-desmethylvenlafaxine. Simultaneous baseline enantiomeric separation of the two compounds was obtained using a mobile phase composed of 100 mM ammonium acetate buffer pH 6/water/acetonitrile (5:5:90, v/v). The electrokinetic injection for sample introduction provided a limit of quantitation for both the compounds of 0.05 microg/ml racemate concentration suitable for the analysis of venlafaxine and metabolite in biological samples. The acetonitrile mobile phase concentration was found to modulate the analytes elution times, the enantiomeric resolution and the efficiency of the separation. The column was tested for repeatability and linearity showing RSD values (%) in the range of 0.13-0.24, 2.47-3.66 and 1.35-2.50 for migration time, sample/internal standard peak area ratio and enantiomeric resolution, respectively and correlation coefficients higher than 0.9990. The method was applied to the analysis of clinical samples of patients under depression therapy showing a stereoselective metabolism for venlafaxine.

  16. Does competence mediate the associations between puberty and internalizing or externalizing problems in adolescent girls?

    PubMed

    Negriff, Sonya; Hillman, Jennifer B; Dorn, Lorah D

    2011-10-01

    To examine separate mediational models linking (a) menarcheal status or (b) pubertal timing to internalizing and externalizing problems through competence. This study involved cross-sectional analyses of 262 adolescent girls (age: 11-17 years; mean = 14.93, standard deviation = 2.17) enrolled in a longitudinal study examining the association of psychological functioning and smoking with reproductive and bone health. Measures of menarcheal status (pre/post), pubertal timing (early, on-time, or late), internalizing and externalizing behavior, and perceived competence (parent and adolescent report) were obtained. Structural equation modeling was used for analyses. Perceived competence was found to fully mediate the association between menarcheal status and parent report of internalizing and externalizing problems. For adolescent report, there was a full mediation effect for internalizing problems but a partial mediation effect for externalizing problems. Being menarcheal was related to lower competence, which was in turn related to higher internalizing and externalizing problems. Models including pubertal timing were not significant. Perceived competence is important in understanding the associations between menarcheal status and internalizing and externalizing problems. Interventions targeting competence, particularly in postmenarcheal girls, may reduce or prevent problem behaviors. Copyright © 2011 Society for Adolescent Health and Medicine. Published by Elsevier Inc. All rights reserved.

  17. Systems and methods for separating a multiphase fluid

    NASA Technical Reports Server (NTRS)

    Weislogel, Mark M. (Inventor); Thomas, Evan A. (Inventor); Graf, John C. (Inventor)

    2011-01-01

    Apparatus and methods for separating a fluid are provided. The apparatus can include a separator and a collector having an internal volume defined at least in part by one or more surfaces narrowing toward a bottom portion of the volume. The separator can include an exit port oriented toward the bottom portion of the volume. The internal volume can receive a fluid expelled from the separator into a flow path in the collector and the flow path can include at least two directional transitions within the collector.

  18. 40 CFR 61.347 - Standards: Oil-water separators.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 9 2012-07-01 2012-07-01 false Standards: Oil-water separators. 61.347 Section 61.347 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS National Emission Standard for Benzene...

  19. Liquid-liquid extraction of strongly protein bound BMS-299897 from human plasma and cerebrospinal fluid, followed by high-performance liquid chromatography/tandem mass spectrometry.

    PubMed

    Xue, Y J; Pursley, Janice; Arnold, Mark

    2007-04-11

    BMS-299897 is a gamma-secretase inhibitor that is being developed for the treatment of Alzheimer's disease. Liquid-liquid extraction (LLE), chromatographic/tandem mass spectrometry (LC/MS/MS) methods have been developed and validated for the quantitation of BMS-299897 in human plasma and cerebrospinal fluid (CSF). Both methods utilized (13)C6-BMS-299897, the stable label isotope analog, as the internal standard. For the human plasma extraction method, two incubation steps were required after the addition of 5 mM ammonium acetate and the internal standard in acetonitrile to release the analyte bound to proteins prior to LLE with toluene. For the human CSF extraction method, after the addition of 0.5 N HCl and the internal standard, CSF samples were extracted with toluene and no incubation was required. The organic layers obtained from both extraction methods were removed and evaporated to dryness. The residues were reconstituted and injected into the LC/MS/MS system. Chromatographic separation was achieved isocratically on a MetaChem C18 Hypersil BDS column (2.0 mm x 50 mm, 3 microm). The mobile phase contained 10 mM ammonium acetate pH 5 and acetonitrile. Detection was by negative ion electrospray tandem mass spectrometry. The standard curves ranged from 1 to 1000 ng/ml for human plasma and 0.25-100 ng/ml for human CSF. Both standard curves were fitted to a 1/x weighted quadratic regression model. For both methods, the intra-assay precision was within 8.2% CV, the inter-assay precision was within 5.4% CV, and assay accuracy was within +/-7.4% of the nominal values. The validation and sample analysis results demonstrated that both methods had acceptable precision and accuracy across the calibration ranges.

  20. Influence of the Separation of Prescription and Dispensation of Medicine on Its Cost in Japanese Prefectures

    PubMed Central

    Yokoi, Masayuki; Tashiro, Takao

    2014-01-01

    We studied how the separation of dispensing and prescribing of medicines between pharmacies and clinics (the “separation system”) can reduce internal medicine costs. To do so, we obtained publicly available data by searching electronic databases and official web pages of the Japanese government and non-profit public service corporations on the Internet. For Japanese medical institutions, participation in the separation system is optional. Consequently, the expansion rate of the separation system for each of the administrative districts is highly variable. The data were subjected to multiple regression analysis; daily internal medicines were the objective variable and expansion rate of the separation system was the explanatory variable. A multiple regression analysis revealed that the expansion rate of the separation system and the rate of replacing brand name medicine with generic medicine showed a significant negative partial correlation with daily internal medicine costs. Thus, the separation system was as effective in reducing medicine costs as the use of generic medicines. Because of its medical economic efficiency, the separation system should be expanded, especially in Asian countries in which the system is underdeveloped. PMID:24999122

  1. Influence of the separation of prescription and dispensation of medicine on its cost in Japanese prefectures.

    PubMed

    Yokoi, Masayuki; Tashiro, Takao

    2014-04-07

    We studied how the separation of dispensing and prescribing of medicines between pharmacies and clinics (the "separation system") can reduce internal medicine costs. To do so, we obtained publicly available data by searching electronic databases and official web pages of the Japanese government and non-profit public service corporations on the Internet. For Japanese medical institutions, participation in the separation system is optional. Consequently, the expansion rate of the separation system for each of the administrative districts is highly variable. The data were subjected to multiple regression analysis; daily internal medicines were the objective variable and expansion rate of the separation system was the explanatory variable. A multiple regression analysis revealed that the expansion rate of the separation system and the rate of replacing brand name medicine with generic medicine showed a significant negative partial correlation with daily internal medicine costs. Thus, the separation system was as effective in reducing medicine costs as the use of generic medicines. Because of its medical economic efficiency, the separation system should be expanded, especially in Asian countries in which the system is underdeveloped.

  2. Extraction of Oleic Acid from Moroccan Olive Mill Wastewater

    PubMed Central

    Elkacmi, Reda; Kamil, Noureddine; Bennajah, Mounir; Kitane, Said

    2016-01-01

    The production of olive oil in Morocco has recently grown considerably for its economic and nutritional importance favored by the country's climate. After the extraction of olive oil by pressing or centrifuging, the obtained liquid contains oil and vegetation water which is subsequently separated by decanting or centrifugation. Despite its treatment throughout the extraction process, this olive mill wastewater, OMW, still contains a very important oily residue, always regarded as a rejection. The separated oil from OMW can not be intended for food because of its high acidity of 3.397% which exceeds the international standard for human consumption defined by the standard of the Codex Alimentarius, proving its poor quality. This work gives value addition to what would normally be regarded as waste by the extraction of oleic acid as a high value product, using the technique of inclusion with urea for the elimination of saturated and unsaturated fatty acids through four successive crystallizations at 4°C and 20°C to have a final phase with oleic acid purity of 95.49%, as a biodegradable soap and a high quality glycerin will be produced by the reaction of saponification and transesterification. PMID:26933663

  3. Extraction of Oleic Acid from Moroccan Olive Mill Wastewater.

    PubMed

    Elkacmi, Reda; Kamil, Noureddine; Bennajah, Mounir; Kitane, Said

    2016-01-01

    The production of olive oil in Morocco has recently grown considerably for its economic and nutritional importance favored by the country's climate. After the extraction of olive oil by pressing or centrifuging, the obtained liquid contains oil and vegetation water which is subsequently separated by decanting or centrifugation. Despite its treatment throughout the extraction process, this olive mill wastewater, OMW, still contains a very important oily residue, always regarded as a rejection. The separated oil from OMW can not be intended for food because of its high acidity of 3.397% which exceeds the international standard for human consumption defined by the standard of the Codex Alimentarius, proving its poor quality. This work gives value addition to what would normally be regarded as waste by the extraction of oleic acid as a high value product, using the technique of inclusion with urea for the elimination of saturated and unsaturated fatty acids through four successive crystallizations at 4°C and 20°C to have a final phase with oleic acid purity of 95.49%, as a biodegradable soap and a high quality glycerin will be produced by the reaction of saponification and transesterification.

  4. Fast Simultaneous Determination of 13 Nucleosides and Nucleobases in Cordyceps sinensis by UHPLC-ESI-MS/MS.

    PubMed

    Zong, Shi-Yu; Han, Han; Wang, Bing; Li, Ning; Dong, Tina Ting-Xia; Zhang, Tong; Tsim, Karl W K

    2015-12-04

    A reliable ultra-high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UHPLC-ESI-MS/MS) method for the fast simultaneous determination of 13 nucleosides and nucleobases in Cordyceps sinensis (C. sinensis) with 2-chloroadenosine as internal standard was developed and validated. Samples were ultrasonically extracted in an ice bath thrice, and the optimum analyte separation was performed on an ACQUITY UPLC(TM) HSS C18 column (100 mm × 2.1 mm, 1.8 μm) with gradient elution. All targeted analytes were separated in 5.5 min. Furthermore, all calibration curves showed good linear regression (r > 0.9970) within the test ranges, and the limits of quantitation and detection of the 13 analytes were less than 150 and 75 ng/mL, respectively. The relative standard deviations (RSDs) of intra- and inter-day precisions were <6.23%. Recoveries of the quantified analytes ranged within 85.3%-117.3%, with RSD < 6.18%. The developed UHPLC-ESI-MS/MS method was successfully applied to determine nucleosides and nucleobases in 11 batches of C. sinensis samples from different regions in China. The range for the total content in the analyzed samples was 1329-2057 µg/g.

  5. A real time quality control application for animal production by image processing.

    PubMed

    Sungur, Cemil; Özkan, Halil

    2015-11-01

    Standards of hygiene and health are of major importance in food production, and quality control has become obligatory in this field. Thanks to rapidly developing technologies, it is now possible for automatic and safe quality control of food production. For this purpose, image-processing-based quality control systems used in industrial applications are being employed to analyze the quality of food products. In this study, quality control of chicken (Gallus domesticus) eggs was achieved using a real time image-processing technique. In order to execute the quality control processes, a conveying mechanism was used. Eggs passing on a conveyor belt were continuously photographed in real time by cameras located above the belt. The images obtained were processed by various methods and techniques. Using digital instrumentation, the volume of the eggs was measured, broken/cracked eggs were separated and dirty eggs were determined. In accordance with international standards for classifying the quality of eggs, the class of separated eggs was determined through a fuzzy implication model. According to tests carried out on thousands of eggs, a quality control process with an accuracy of 98% was possible. © 2014 Society of Chemical Industry.

  6. 33 CFR 155.380 - Oily water separating equipment and bilge alarm approval standards.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... PREVENTION REGULATIONS FOR VESSELS Vessel Equipment § 155.380 Oily water separating equipment and bilge alarm approval standards. (a) On U.S. inspected ships, oily water separating equipment and bilge alarms must be... routine maintenance of the oily water separating equipment and the bilge alarm must be clearly defined by...

  7. 33 CFR 155.380 - Oily water separating equipment and bilge alarm approval standards.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... PREVENTION REGULATIONS FOR VESSELS Vessel Equipment § 155.380 Oily water separating equipment and bilge alarm approval standards. (a) On U.S. inspected ships, oily water separating equipment and bilge alarms must be... routine maintenance of the oily water separating equipment and the bilge alarm must be clearly defined by...

  8. 33 CFR 155.380 - Oily water separating equipment and bilge alarm approval standards.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... PREVENTION REGULATIONS FOR VESSELS Vessel Equipment § 155.380 Oily water separating equipment and bilge alarm approval standards. (a) On U.S. inspected ships, oily water separating equipment and bilge alarms must be... routine maintenance of the oily water separating equipment and the bilge alarm must be clearly defined by...

  9. 33 CFR 155.380 - Oily water separating equipment and bilge alarm approval standards.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... PREVENTION REGULATIONS FOR VESSELS Vessel Equipment § 155.380 Oily water separating equipment and bilge alarm approval standards. (a) On U.S. inspected ships, oily water separating equipment and bilge alarms must be... routine maintenance of the oily water separating equipment and the bilge alarm must be clearly defined by...

  10. Current situation of International Organization for Standardization/Technical Committee 249 international standards of traditional Chinese medicine.

    PubMed

    Liu, Yu-Qi; Wang, Yue-Xi; Shi, Nan-Nan; Han, Xue-Jie; Lu, Ai-Ping

    2017-05-01

    To review the current situation and progress of traditional Chinese medicine (TCM) international standards, standard projects and proposals in International Organization for Standardization (ISO)/ technical committee (TC) 249. ISO/TC 249 standards and standard projects on the ISO website were searched and new standard proposals information were collected from ISO/TC 249 National Mirror Committee in China. Then all the available data were summarized in 5 closely related items, including proposed time, proposed country, assigned working group (WG), current stage and classifification. In ISO/TC 249, there were 2 international standards, 18 standard projects and 24 new standard proposals proposed in 2014. These 44 standard subjects increased year by year since 2011. Twenty-nine of them were proposed by China, 15 were assigned to WG 4, 36 were in preliminary and preparatory stage and 8 were categorized into 4 fifields, 7 groups and sub-groups based on International Classifification Standards. A rapid and steady development of international standardization in TCM can be observed in ISO/TC 249.

  11. Quantification of Paclitaxel and Polyaspartate Paclitaxel Conjugate in Beagle Plasma: Application to a Pharmacokinetic Study.

    PubMed

    Gao, Yangyang; Chen, Junying; Zhang, Xiqian; Xie, Huiru; Wang, Yanran; Guo, Shuquan

    2017-03-01

    An LC-MS/MS method for the determination of polyaspartate paclitaxel conjugate (PASP-PTX) and paclitaxel (PTX) in dog plasma with cephalomannine (Internal Standard for PASP-PTX, IS-I) and clopidogrel bisulfate (Internal Standard for PTX, IS-II) as the internal standards was developed and validated. Plasma samples of PASP-PTX were extracted by ethyl acetate following the hydrolysis reaction, while protein precipitation was used for the extraction of PTX using acetonitrile. Analytes were separated by a CAPCELL PAK C18 MG II column using a gradient elution with the mobile phase (A) 5 mM ammonium containing 0.1% formic acid, and (B) acetonitrile. Quantification was performed by monitoring the m/z transitions of 286.2/105.0 for PASP-PTX, 264.2/83.0 for IS-I, 854.4/286.0 for PTX, and 322.1/184.1 for IS-II in the ESI positive mode. This method was validated in terms of specificity, linearity, precision, accuracy, and stability. The lower limit of quantification was 0.15 µg/mL for PASP-PTX and 0.01 µg/mL for PTX, and the calibration curves were linear over 0.15-300 µg/mL for PASP-PTX and over 0.01-10 µg/mL for PTX. The samples were stable under all the tested conditions. The method was successfully applied to study the pharmacokinetic profiles of PASP-PTX and PTX in beagles following intravenous administration of PASP-PTX. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  12. Significant improvements in the practice patterns of adult related donor care in US transplant centers

    PubMed Central

    MBChB, Chloe Anthias; Shaw, Bronwen E; Kiefer, Deidre M; Liesveld, Jane L; Yared, Jean; Kambl, Rammurti T; D'Souza, Anita; Hematti, Peiman; Seftel, Matthew D; Norkin, Maxim; DeFilipp, Zachariah M; Kasow, Kimberly A; Abidi, Muneer H; Savani, Bipin N; Shah, Nirali N; Anderlini, Paolo; Diaz, Miguel A; Malone, Adriana K; Halter, Joerg P; Lazarus, Hillard M; Logan, Brent R; Switzer, Galen E; Pulsipher, Michael A; Confer, Dennis L; O'Donnell, Paul V

    2016-01-01

    Recent investigations have found a higher incidence of adverse events associated with hematopoietic cell donation in related donors (RDs) who have morbidities that if present in an unrelated donor (UD) would preclude donation. In the UD setting, regulatory standards ensure independent assessment of donors, one of several crucial measures to safeguard donor health and safety. A survey conducted by the Center for International Blood and Marrow Transplant Research (CIBMTR) Donor Health and Safety Working Committee in 2007 reported a potential conflict of interest in >70% US centers, where physicians had simultaneous responsibility for RDs and their recipients. Consequently, several international organizations have endeavored to improve practice through regulations and consensus recommendations. We hypothesized that the changes in the 2012 FACT-JACIE Standards, resulting from the CIBMTR study, will have significantly impacted practice. Accordingly, a follow-up survey of US transplant centers was conducted to assess practice changes since 2007, and investigate additional areas where RD care was predicted to differ from UD care. 73 centers (53%), performing 79% of US RD transplants responded. Significant improvements were observed since the earlier survey; 62% centers now ensure separation of RD and recipient care (P<0.0001). However, this study identifies several areas where RD management does not meet international donor care standards. Particular concerns include counseling and assessment of donors before HLA typing, with 61% centers first disclosing donor HLA results to an individual other than the donor, the use of unlicensed mobilization agents, and the absence of long-term donor follow-up. Recommendations for improvement are described. PMID:26597080

  13. Quantification of 16 polycyclic aromatic hydrocarbons in cigarette smoke condensate using stable isotope dilution liquid chromatography with atmospheric-pressure photoionization tandem mass spectrometry.

    PubMed

    Zhang, Xiaotao; Hou, Hongwei; Chen, Huan; Liu, Yong; Wang, An; Hu, Qingyuan

    2015-09-17

    A stable isotope dilution liquid chromatography with tandem mass spectrometry method for the analysis of 16 polycyclic aromatic hydrocarbons in cigarette smoke condensate was developed and validated. Compared with previously reported methods, this method has lower limits of detection (0.04-1.35 ng/cig). Additionally, the proposed method saves time, reduces the number of separation steps, and reduces the quantity of solvent needed. The new method was applied to evaluate polycyclic aromatic hydrocarbon content in 213 commercially available cigarettes in China, under the International Standardization Organization smoking regime and the Health Canadian intense smoking regime. The results showed that the total polycyclic aromatic hydrocarbon content was more than two times higher in samples from the Health Canadian intense smoking regime than in samples from the International Standardization Organization smoking regime (1189.23 vs. 2859.50 ng/cig, p<0.05). Meanwhile, the concentration of individual polycyclic aromatic hydrocarbons (and total polycyclic aromatic hydrocarbons) increased with labeled tar content in both of the tested smoking regimes. There was a positive correlation between total polycyclic aromatic hydrocarbons under the International Standardization Organization smoking regime with that under the Health Canadian intense smoking regime. The proposed liquid chromatography with tandem mass spectrometry method is satisfactory for the rapid, sensitive, and accurately quantitative evaluation of polycyclic aromatic hydrocarbon content in cigarette smoke condensate, and it can be applied to assess potential health risks from smoking. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  14. An international project to confirm Soviet-era results on immunological and teratological effects of RF field exposure in Wistar rats and comments on Grigoriev et al. [2010].

    PubMed

    Repacholi, Michael; Buschmann, Jochen; Pioli, Claudio; Sypniewska, Roza

    2011-05-01

    Results of key Soviet-era studies dealing with effects on the immune system and teratological consequences in rats exposed to radiofrequency (RF) fields serve, in part, as a basis for setting exposure limits in the USSR and the current RF standards in Russia. The World Health Organization's (WHO) International EMF Project considered these Soviet results important enough that they should be confirmed using more modern methods. Since the Soviet papers did not contain comprehensive details on how the results were obtained, Professor Yuri Grigoriev worked with Dr. Bernard Veyret to agree on the final study protocol and to conduct separate studies in Moscow and Bordeaux under the same protocol. The International Oversight Committee (IOC) provided oversight on the conduct of the studies and was the firewall committee that dealt with the sponsors and researchers. This paper gives the IOC comments and conclusions on the differing results between the two studies. Copyright © 2010 Wiley-Liss, Inc.

  15. Interoperability In The New Planetary Science Archive (PSA)

    NASA Astrophysics Data System (ADS)

    Rios, C.; Barbarisi, I.; Docasal, R.; Macfarlane, A. J.; Gonzalez, J.; Arviset, C.; Grotheer, E.; Besse, S.; Martinez, S.; Heather, D.; De Marchi, G.; Lim, T.; Fraga, D.; Barthelemy, M.

    2015-12-01

    As the world becomes increasingly interconnected, there is a greater need to provide interoperability with software and applications that are commonly being used globally. For this purpose, the development of the new Planetary Science Archive (PSA), by the European Space Astronomy Centre (ESAC) Science Data Centre (ESDC), is focused on building a modern science archive that takes into account internationally recognised standards in order to provide access to the archive through tools from third parties, for example by the NASA Planetary Data System (PDS), the VESPA project from the Virtual Observatory of Paris as well as other international institutions. The protocols and standards currently being supported by the new Planetary Science Archive at this time are the Planetary Data Access Protocol (PDAP), the EuroPlanet-Table Access Protocol (EPN-TAP) and Open Geospatial Consortium (OGC) standards. The architecture of the PSA consists of a Geoserver (an open-source map server), the goal of which is to support use cases such as the distribution of search results, sharing and processing data through a OGC Web Feature Service (WFS) and a Web Map Service (WMS). This server also allows the retrieval of requested information in several standard output formats like Keyhole Markup Language (KML), Geography Markup Language (GML), shapefile, JavaScript Object Notation (JSON) and Comma Separated Values (CSV), among others. The provision of these various output formats enables end-users to be able to transfer retrieved data into popular applications such as Google Mars and NASA World Wind.

  16. 40 CFR 63.7910 - What emissions limitations and work practice standards must I meet for separators?

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS... Pollutants: Site Remediation Separators § 63.7910 What emissions limitations and work practice standards must...

  17. 40 CFR 63.7910 - What emissions limitations and work practice standards must I meet for separators?

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS... Pollutants: Site Remediation Separators § 63.7910 What emissions limitations and work practice standards must...

  18. 40 CFR 63.7910 - What emissions limitations and work practice standards must I meet for separators?

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS... Pollutants: Site Remediation Separators § 63.7910 What emissions limitations and work practice standards must...

  19. 40 CFR 63.7910 - What emissions limitations and work practice standards must I meet for separators?

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS... Pollutants: Site Remediation Separators § 63.7910 What emissions limitations and work practice standards must...

  20. 40 CFR 63.7910 - What emissions limitations and work practice standards must I meet for separators?

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS... Pollutants: Site Remediation Separators § 63.7910 What emissions limitations and work practice standards must...

  1. Collaborative study on saccharide quantification of the Haemophilus influenzae type b component in liquid vaccine presentations.

    PubMed

    Rosskopf, U; Daas, A; Terao, E; von Hunolstein, C

    2017-01-01

    Before release onto the market, it must be demonstrated that the total and free polysaccharide (poly ribosyl-ribitol-phosphate, PRP) content of Haemophilus influenzae type b (Hib) vaccine complies with requirements. However, manufacturers use different methods to assay PRP content: a national control laboratory must establish and validate the relevant manufacturer methodology before using it to determine PRP content. An international study was organised by the World Health Organization (WHO), in collaboration with the Biological Standardisation Programme (BSP) of the Council of Europe/European Directorate for the Quality of Medicines & HealthCare (EDQM) and of the European Union Commission, to verify the suitability of a single method for determining PRP content in liquid pentavalent vaccines (DTwP-HepB-Hib) containing a whole-cell pertussis component. It consists of HCl hydrolysis followed by chromatographic separation and quantification of ribitol on a CarboPac MA1 column using high-performance anion exchange chromatography coupled with pulsed amperometric detection (HPAEC-PAD). The unconjugated, free, PRP is separated from the total PRP using C4 solid-phase extraction cartridges (SPE C4). Ten quality control laboratories performed two independent analyses applying the proposed analytical test protocol to five vaccine samples, including a vaccine lot with sub-potent PRP content and very high free PRP content. Both WHO PRP standard and ribitol reference standard were included as calibrating standards. A significant bias between WHO PRP standard and ribitol reference standard was observed. Study results showed that the proposed analytical method is, in principle, suitable for the intended use provided that a validation is performed as usually expected from quality control laboratories.

  2. A complete ray-trace analysis of the Mirage toy

    NASA Astrophysics Data System (ADS)

    Adhya, Sriya; Noé, John W.

    2007-06-01

    The `Mirage' (Opti-Gone International) is a well-known optics demonstration (PIRA index number 6A20.35) that uses two opposed concave mirrors to project a real image of a small object into space. We studied image formation in the Mirage by standard 2x2 matrix methods and by exact ray tracing, with particular attention to additional real images that can be observed when the mirror separation is increased beyond one focal length. We find that the three readily observed secondary images correspond to 4, 6, or 8 reflections, respectively, contrary to previous reports.

  3. Green chromatography separation of analytes of greatly differing properties using a polyethylene glycol stationary phase and a low-toxic water-based mobile phase.

    PubMed

    Šatínský, Dalibor; Brabcová, Ivana; Maroušková, Alena; Chocholouš, Petr; Solich, Petr

    2013-07-01

    A simple, rapid, and environmentally friendly HPLC method was developed and validated for the separation of four compounds (4-aminophenol, caffeine, paracetamol, and propyphenazone) with different chemical properties. A "green" mobile phase, employing water as the major eluent, was proposed and applied to the separation of analytes with different polarity on polyethylene glycol (PEG) stationary phase. The chromatography separation of all compounds and internal standard benzoic acid was performed using isocratic elution with a low-toxicity mobile phase consisting of 0.04% (v/v) triethylamine and water. HPLC separation was carried out using a PEG reversed-phase stationary phase Supelco Discovery HS PEG column (15 × 4 mm; particle size 3 μm) at a temperature of 30 °C and flow rate at 1.0 mL min(-1). The UV detector was set at 210 nm. In this study, a PEG stationary phase was shown to be suitable for the efficient isocratic separation of compounds that differ widely in hydrophobicity and acid-base properties, particularly 4-aminophenol (log P, 0.30), caffeine (log P, -0.25), and propyphenazone (log P, 2.27). A polar PEG stationary phase provided specific selectivity which allowed traditional chromatographic problems related to the separation of analytes with different polarities to be solved. The retention properties of the group of structurally similar substances (aromatic amines, phenolic compounds, and xanthine derivatives) were tested with different mobile phases. The proposed green chromatography method was successfully applied to the analysis of active substances and one degradation impurity (4-aminophenol) in commercial preparation. Under the optimum chromatographic conditions, standard calibration was carried out with good linearity correlation coefficients for all compounds in the range (0.99914-0.99997, n = 6) between the peak areas and concentration of compounds. Recovery of the sample preparation was in the range 100 ± 5% for all compounds. The intraday method precision was determined as RSD, and the values were lower than 1.00%.

  4. Simultaneous Separation of Acidic and Basic Isoperoxidases in Wounded Potato Tissue by Acrylamide Gel Electrophoresis 1

    PubMed Central

    Borchert, Rolf; Decedue, Charles J.

    1978-01-01

    Preparation and use of a newly developed pH 4.3 horizontal thin layer acrylamide gel which permits the simultaneous separation of acidic and basic isoperoxidases in up to 30 samples is described. Use of cytochrome c, horseradish peroxidase, and a purified potato isoperoxidase as internal standards for a range in isoelectric points of peroxidases from pH 3 to 11 is introduced to facilitate comparison of results obtained with different materials and different methods. Distribution of tissue-specific isoperoxidases in different cell layers of wounded potato (Solanum tuberosum L.) tissue is shown and their purification described. Evidence for the in vitro degradation of basic potato isoperoxidases resulting in more acidic forms similar to isoperoxidases occurring in wounded potato tissue is presented. The significance of this observation for the postulated differential function of different isoperoxidases is discussed. ImagesFig. 1-3 PMID:16660608

  5. 26 CFR 1.4-3 - Husband and wife filing separate returns.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... Section 1.4-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY INCOME TAX INCOME TAXES Normal Taxes and Surtaxes § 1.4-3 Husband and wife filing separate returns. (a) In general. If the... each elect to pay the optional tax imposed under section 3 or neither may so elect. If the separate...

  6. Application of a Fast Separation Method for Anti-diabetics in Pharmaceuticals Using Monolithic Column: Comparative Study With Silica Based C-18 Particle Packed Column.

    PubMed

    Hemdan, A; Abdel-Aziz, Omar

    2018-04-01

    Run time is a predominant factor in HPLC for quality control laboratories especially if there is large number of samples have to be analyzed. Working at high flow rates cannot be attained with silica based particle packed column due to elevated backpressure issues. The use of monolithic column as an alternative to traditional C-18 column was tested for fast separation of pharmaceuticals, where the results were very competitive. The performance comparison of both columns was tested for separation of anti-diabetic combination containing Metformin, Pioglitazone and Glimepiride using Gliclazide as an internal standard. Working at high flow rates with less significant backpressure was obtained with the monolithic column where the run time was reduced from 6 min in traditional column to only 1 min in monolithic column with accepted resolution. The structure of the monolith contains many pores which can adapt the high flow rate of the mobile phase. Moreover, peak symmetry and equilibration time were more efficient with monolithic column.

  7. Determination of the complete structure of natural lecithins.

    PubMed

    Kuksis, A; Marai, L

    1967-05-01

    A method is described for the separation, identification, and quantitative estimation of the individual molecular species occurring in natural lecithin mixtures. Purified lecithin preparations are converted into diglyceride acetates by enzymic dephosphorylation and acetylation. The diglyceride acetates are separated on the basis of the degree of unsaturation and the molecular geometry by means of chromatography on thin layers of silica gel which are impregnated with silver nitrate. The various acetates thus resolved are separately recovered from the plates and diluted with tridecanoin internal standard; the quantitative distribution of the molecular weights is determined by gas chromatography.Suitable aliquots of the saturated and unsaturated diglyceride acetates are further analyzed for over-all and for positional distribution of fatty acids. The identity and proportions of the various lecithins are deduced by integration and normalization of all the experimental data. Where doubt exists, specific diglyceride acetates are isolated by preparative gas chromatography, and their fatty acid composition is determined. The method is illustrated with data obtained for the mixed lecithins of egg yolk. The general approach is applicable to the determination of the structure of other phospholipids of comparable complexity.

  8. Quantification of apolipoprotein B-48 and B-100 in rat liver endoplasmic reticulum and Golgi fractions.

    PubMed Central

    Cartwright, I J; Higgins, J A

    1992-01-01

    We have developed a method for measurement of apolipoprotein (apo) B-48 and apo B-100 in blood and subcellular fractions of rat liver based on SDS/PAGE followed by quantitative immunoblotting using 125I-Protein A. Standard curves were prepared in each assay using apo B prepared from total rat lipoproteins by extraction with tetramethylurea. Subcellular fractions (rough and smooth endoplasmic reticulum and Golgi fractions) were prepared from rat liver and separated into membrane and cisternal-content fractions. For quantification, membrane fractions were solubilized in Triton X-100, and the apo B was immunoprecipitated before separation by SDS/PAGE and immunoblotting. Content fractions were concentrated by ultrafiltration and separated by SDS/PAGE without immunoprecipitation. Quantification of apo B in subcellular fractions and detection of apo B by immunoblotting yielded consistent results. In all fractions apo B-48 was the major form, accounting for approximately three-quarters of the total apo B. By using marker enzymes as internal standards, it was calculated that all of the apo B was recovered in the endoplasmic reticulum and Golgi fractions, with approximately 80% of each form of apo B in the endoplasmic reticulum. More than 90% of the apo B of the rough- and smooth-endoplasmic-reticulum fractions was membrane-bound, whereas approx. 33 and 15% of the apo B of the cis-enriched Golgi fractions and trans-enriched Golgi fractions respectively were membrane-bound. Images Fig. 1. Fig. 3. Fig. 4. PMID:1637294

  9. 75 FR 19944 - International Code Council: The Update Process for the International Codes and Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2010-04-16

    ... for Residential Construction in High Wind Areas. ICC 700: National Green Building Standard. The... Codes and Standards that are comprehensive, coordinated, and necessary to regulate the built environment... International Codes and Standards consist of the following: ICC Codes International Building Code. International...

  10. Determination of boron in uranium aluminum silicon alloy by spectrophotometry and estimation of expanded uncertainty in measurement

    NASA Astrophysics Data System (ADS)

    Ramanjaneyulu, P. S.; Sayi, Y. S.; Ramakumar, K. L.

    2008-08-01

    Quantification of boron in diverse materials of relevance in nuclear technology is essential in view of its high thermal neutron absorption cross section. A simple and sensitive method has been developed for the determination of boron in uranium-aluminum-silicon alloy, based on leaching of boron with 6 M HCl and H 2O 2, its selective separation by solvent extraction with 2-ethyl hexane 1,3-diol and quantification by spectrophotometry using curcumin. The method has been evaluated by standard addition method and validated by inductively coupled plasma-atomic emission spectroscopy. Relative standard deviation and absolute detection limit of the method are 3.0% (at 1 σ level) and 12 ng, respectively. All possible sources of uncertainties in the methodology have been individually assessed, following the International Organization for Standardization guidelines. The combined uncertainty is calculated employing uncertainty propagation formulae. The expanded uncertainty in the measurement at 95% confidence level (coverage factor 2) is 8.840%.

  11. Sensitive and selective liquid chromatography-tandem mass spectrometry method for the quantification of aniracetam in human plasma.

    PubMed

    Zhang, Jingjing; Liang, Jiabi; Tian, Yuan; Zhang, Zunjian; Chen, Yun

    2007-10-15

    A rapid, sensitive and selective LC-MS/MS method was developed and validated for the quantification of aniracetam in human plasma using estazolam as internal standard (IS). Following liquid-liquid extraction, the analytes were separated using a mobile phase of methanol-water (60:40, v/v) on a reverse phase C18 column and analyzed by a triple-quadrupole mass spectrometer in the selected reaction monitoring (SRM) mode using the respective [M+H]+ ions, m/z 220-->135 for aniracetam and m/z 295-->205 for the IS. The assay exhibited a linear dynamic range of 0.2-100 ng/mL for aniracetam in human plasma. The lower limit of quantification (LLOQ) was 0.2 ng/mL with a relative standard deviation of less than 15%. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. The validated LC-MS/MS method has been successfully applied to study the pharmacokinetics of aniracetam in healthy male Chinese volunteers.

  12. Determination of the rare-earth elements in geological materials by inductively coupled plasma mass spectrometry

    USGS Publications Warehouse

    Lichte, F.E.; Meier, A.L.; Crock, J.G.

    1987-01-01

    A method of analysis of geological materials for the determination of the rare-earth elements using the Inductively coupled plasma mass spectrometric technique (ICP-MS) has been developed. Instrumental parameters and factors affecting analytical results have been first studied and then optimized. Samples are analyzed directly following an acid digestion, without the need for separation or preconcentration with limits of detection of 2-11 ng/g, precision of ?? 2.5% relative standard deviation, and accuracy comparable to inductively coupled plasma emission spectrometry and instrumental neutron activation analysis. A commercially available ICP-MS instrument is used with modifications to the sample introduction system, torch, and sampler orifice to reduce the effects of high salt content of sample solutions prepared from geologic materials. Corrections for isobaric interferences from oxide ions and other diatomic and triatomic ions are made mathematically. Special internal standard procedures are used to compensate for drift in metahmetal oxide ratios and sensitivity. Reference standard values are used to verify the accuracy and utility of the method.

  13. 26 CFR 1.614-3 - Rules relating to separate operating mineral interests in the case of mines.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 7 2011-04-01 2009-04-01 true Rules relating to separate operating mineral interests in the case of mines. 1.614-3 Section 1.614-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES (CONTINUED) Natural Resources § 1...

  14. 26 CFR 1.414(r)-8 - Separate application of section 410(b).

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 5 2010-04-01 2010-04-01 false Separate application of section 410(b). 1.414(r)-8 Section 1.414(r)-8 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-8...

  15. Examination to assess the clinical examination and documentation of spine pathology among orthopedic residents.

    PubMed

    Haglin, Jack M; Zeller, John L; Egol, Kenneth A; Phillips, Donna P

    2017-12-01

    The Accreditation Council for Graduate Medical Education (ACGME) guidelines requires residency programs to teach and evaluate residents in six overarching "core competencies" and document progress through educational milestones. To assess the progress of orthopedic interns' skills in performing a history, physical examination, and documentation of the encounter for a standardized patient with spinal stenosis, an objective structured clinical examination (OSCE) was conducted for 13 orthopedic intern residents, following a 1-month boot camp that included communications skills and curriculum in history and physical examination. Interns were objectively scored based on their performance of the physical examination, communication skills, completeness and accuracy of their electronic medical record (EMR), and their diagnostic conclusions gleaned from the patient encounter. The purpose of this study was to meaningfully assess the clinical skills of orthopedic post-graduate year (PGY)-1 interns. The findings can be used to develop a standardized curriculum for documenting patient encounters and highlight common areas of weakness among orthopedic interns with regard to the spine history and physical examination and conducting complete and accurate clinical documentation. A major orthopedic specialty hospital and academic medical center. Thirteen PGY-1 orthopedic residents participated in the OSCE with the same standardized patient presenting with symptoms and radiographs consistent with spinal stenosis. Videos of the encounters were independently viewed and objectively evaluated by one investigator in the study. This evaluation focused on the completeness of the history and the performance and completion of the physical examination. The standardized patient evaluated the communication skills of each intern with a separate objective evaluation. Interns completed these same scoring guides to evaluate their own performance in history, physical examination, and communications skills. The interns' documentation in the EMR was then scored for completeness, internal consistency, and inaccuracies. The independent review revealed objective deficits in both the orthopedic interns' history and the physical examination, as well as highlighted trends of inaccurate and incomplete documentation in the corresponding medical record. Communication skills with the patient did not meet expectations. Further, interns tended to overscore themselves, especially with regard to their performance on the physical examination (p<.0005). Inconsistencies, omissions, and inaccuracies were common in the corresponding medical notes when compared with the events of the patient encounter. Nine of the 13 interns (69.2%) documented at least one finding that was not assessed or tested in the clinical encounter, and four of the 13 interns (30.8%) included inaccuracies in the medical record, which contradicted the information collected at the time of the encounter. The results of this study highlighted significant shortcomings in the completeness of the interns' spine history and physical examination, and the accuracy and completeness oftheir EMR note. The study provides a valuable exercise for evaluating residents in a multifaceted, multi-milestone manner that more accurately documents residents' clinical strengths and weaknesses. The study demonstrates that orthopedic residents require further instruction on the complexities of the spinal examination. It validates a need for increased systemic support for improving resident documentation through comprehensive education and evaluation modules. Copyright © 2017 Elsevier Inc. All rights reserved.

  16. 40 CFR 61.352 - Alternative standards for oil-water separators.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 9 2014-07-01 2014-07-01 false Alternative standards for oil-water separators. 61.352 Section 61.352 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS (CONTINUED) NATIONAL EMISSION STANDARDS FOR HAZARDOUS AIR POLLUTANTS National Emission Standard for Benzene Waste Operations § 61.352...

  17. A method for the low-level (ng/g) determination of perfluorooctanoate in carpet by LC-MS-MS using matrix extracted standards.

    PubMed

    L'Empereur, Karen; Stadalius, Marilyn; Zhu, Yongdong; Mansoori, Bashir A; Isemura, Tsuguhide; Kaiser, Mary A; Knaup, Wolfgang; Noguchi, Masahiro

    2008-08-01

    Fluorotelomer-based acrylic polymers are applied to the surface of carpet to impart oil, stain, and water repellence properties. Concerns that fluorotelomer-based polymers are a possible source of "low level" exposure to humans, coupled with their widespread use have prompted the need to develop a method to detect and measure perfluorooctanoate (PFO) in carpet. A liquid chromatography tandem mass spectrometry method for the determination of PFO in carpet using a dual labeled 13C-perfluoroctanoic acid (13C-PFOA) internal standard is successfully developed and validated. Levels of PFO are determined using a gradient, reversed-phase high-performance liquid chromatography (HPLC) method with acetic acid acidified water-methanol, separated on a 50 mm Phenomenex Synergi Polar RP column. Ions monitored are 413 (parent) and 369 (daughter) for PFO and 415 (parent) and 370 (daughter) for dual labeled 13C-PFOA internal standard. Accuracy and precision over three days for 5 to 900 ng/g PFO in carpet ranged from 2.4% to 7.6% and 3.7% to 14.1%, respectively. Overall extraction efficiency for samples (n=30) fortified with 13C-PFOA at 20 ng/g and perfluorooctanoic acid (PFOA) at 5, 50, and 500 ng/g is 98.9%+/-8.1%. Specificity of the method was evaluated with two different carpet samples.

  18. A liquid chromatography method with single quadrupole mass spectrometry for quantitative determination of indomethacin in maternal plasma and urine of pregnant patients

    PubMed Central

    Wang, Xiaoming; Vernikovskaya, Daria I.; Nanovskaya, Tatiana N.; Rytting, Erik; Hankins, Gary D.V.; Ahmed, Mahmoud S.

    2013-01-01

    A liquid chromatography with single quadrupole mass spectrometry method was developed for the quantitative determination of indomethacin in the maternal plasma and urine of pregnant patients under treatment. A deuterium-labeled isotope of indomethacin (d4-indomethacin) was used as an internal standard. The maternal plasma and urine samples were acidified with 1.0 MHCl then extracted with chloroform to achieve the extraction recovery range of 94% to 104% with variation less than 11%. Chromatographic separation was achieved by a Waters Symmetry C18 column with isocratic elution of 0.05% (v/v) formic acid aqueous solution and acetonitrile (47:53, v/v). An in-source fragmentation was applied on the single quadrupole mass spectrometer equipped with an electrospray ionization source at positive mode. The LC-ESI-MS quantification was performed in the selected ion monitoring mode targeting ions at m/z 139 for indomethacin and m/z 143 for its internal standard. The calibration curves were linear in the concentration ranges between 14.8 and 2.97×103 ng/mL for plasma samples and between 10.5 and 4.21×103 ng/mL for urine samples. The relative standard deviation of this method was less than 8% for intra- and inter-day assays, and the accuracy ranged between 90% and 108%. PMID:23474812

  19. [Simultaneous determination of trichloroethylene and trichloroethanol in blood by liquid-liquid extraction-gas chromatography].

    PubMed

    Ye, H P; Shao, J; Tan, S W; Shan, X Y; Shi, Y P

    2017-10-20

    Objective: To establish a method for determing the trichloroethylene(TCE)and trichloroethanol(TCOH)in blood samples by liquid-liquid extraction-gas chromatography with electron capture detector. Methods: With this method,ether was used as extraction solvent and trichloromethane was used as an internal standard. The whole blood sample was extracted with ether, and dehydrated by anhydrous sodium sulfate. Then the analytes were separated on HP-5 capillary column(30m×0.32mm×0.15μm)and detected byECD.The retention time was for qualitative analysis and the internal standard was for quantitation. Results: The standard curves of TCE and TCOH showed significant linearity between 95.5μg/L-7640.0μg/L( r =0.9997)and 19.0μg/L-1520.0μg/L( r =0.9992). The average recovery was 95.5%-103.6%.The intra-day and inter-day precisions( RSD )were 2.5%-6.8%( n =6)and 1.6%-4.3%( n =6) respectively. The detect limit of TCE and TCOH were 2.10 μg/L and 0.56μg/L(S/N=3)respectively.The blood can be kept 7 days at-20℃ refrigerator without significantly loss. Conclusion: This method is proved to be simple,practical and highly sensitive. It can satisfy the request for the determination of blood samples of humans exposed to TCE.

  20. [Separation and determination of eight plant hormones by reversed-phase high performance liquid chromatography].

    PubMed

    Fang, N; Hou, S; Shao, X; He, Y; Zhao, G

    1998-09-01

    In this paper, reversed-phase high performance liquid chromatographic technique was used for the separation and determination of eight plant hormones. Methanol-water-acetic acid system was chosen as the mobile phase. The effects of different separation conditions, such as the methanol and acetic acid concentrations in mobile phase, on the retention behaviours of eight plant hormones in this system were studied. The general trends in retention behaviours could be correlated to the methanol concentration in mobile phase. The experimental results showed that the optimum separation was achieved with following gradient elution condition: 0-3 minutes, 70% (water percentage in mobile phase), 3-13 minutes, 70%-20%, 13-48 minutes, 20%. Benzene was added to be as the internal standard. Under this experimental condition, the eight plant hormones could be separated completely and detected quantitatively at 260 nm within 16 minutes. The calibration curves for the eight compounds gave linearity over a wide range. The correlation coefficients of each components were r(ZT) = 0.9971, r(GAs) = 0.9999, r(K) = 0.9997, r(BA) = 0.9995, r(IAA) = 0.9998, r(IPA) = 0.9982, r(IBA) = 0.9995 and r(NAA) = 0.9995. The method is rapid, simple and efficient. It is a suitable method for the accurate determination of gibberellic acid (GA) and alpha-naphthaleneacetic acid (alpha-NAA) in products for agricultural use.

  1. 25 CFR 542.32 - What are the minimum internal control standards for internal audit for Tier B gaming operations?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for internal audit for Tier B gaming operations? 542.32 Section 542.32 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.32 What are the minimum internal control standards for...

  2. 25 CFR 542.22 - What are the minimum internal control standards for internal audit for Tier A gaming operations?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 2 2012-04-01 2012-04-01 false What are the minimum internal control standards for internal audit for Tier A gaming operations? 542.22 Section 542.22 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.22 What are the minimum internal control standards for...

  3. 25 CFR 542.22 - What are the minimum internal control standards for internal audit for Tier A gaming operations?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for internal audit for Tier A gaming operations? 542.22 Section 542.22 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.22 What are the minimum internal control standards for...

  4. 25 CFR 542.22 - What are the minimum internal control standards for internal audit for Tier A gaming operations?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for internal audit for Tier A gaming operations? 542.22 Section 542.22 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.22 What are the minimum internal control standards for...

  5. 25 CFR 542.22 - What are the minimum internal control standards for internal audit for Tier A gaming operations?

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 25 Indians 2 2011-04-01 2011-04-01 false What are the minimum internal control standards for internal audit for Tier A gaming operations? 542.22 Section 542.22 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.22 What are the minimum internal control standards for...

  6. 25 CFR 542.32 - What are the minimum internal control standards for internal audit for Tier B gaming operations?

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 25 Indians 2 2011-04-01 2011-04-01 false What are the minimum internal control standards for internal audit for Tier B gaming operations? 542.32 Section 542.32 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.32 What are the minimum internal control standards for...

  7. 25 CFR 542.32 - What are the minimum internal control standards for internal audit for Tier B gaming operations?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 2 2012-04-01 2012-04-01 false What are the minimum internal control standards for internal audit for Tier B gaming operations? 542.32 Section 542.32 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.32 What are the minimum internal control standards for...

  8. 25 CFR 542.32 - What are the minimum internal control standards for internal audit for Tier B gaming operations?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for internal audit for Tier B gaming operations? 542.32 Section 542.32 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.32 What are the minimum internal control standards for...

  9. Analysis of carvedilol enantiomers in human plasma using chiral stationary phase column and liquid chromatography with tandem mass spectrometry.

    PubMed

    Poggi, Josiane Cristófani; Da Silva, Flávia Garcez; Coelho, Eduardo Barbosa; Marques, Maria Paula; Bertucci, Carlo; Lanchote, Vera Lucia

    2012-03-01

    Carvedilol is an antihypertensive drug available as a racemic mixture. (-)-(S)-carvedilol is responsible for the nonselective β-blocker activity but both enantiomers present similar activity on α(1)-adrenergic receptor. To our knowledge, this is the first study of carvedilol enantiomers in human plasma using a chiral stationary phase column and liquid chromatography with tandem mass spectrometry. The method involves plasma extraction with diisopropyl ether using metoprolol as internal standard and direct separation of the carvedilol enantiomers on a Chirobiotic T® (Teicoplanin) column. Protonated ions [M + H](+) and their respective ion products were monitored at transitions of 407 > 100 for the carvedilol enantiomers and 268 > 116 for the internal standard. The quantification limit was 0.2 ng ml(-1) for both enantiomers in plasma. The method was applied to study enantioselectivity in the pharmacokinetics of carvedilol administered as a single dose of 25 mg to a hypertensive patient. The results showed a higher plasma concentration of (+)-(R)-carvedilol (AUC(0-∞) 205.52 vs. 82.61 (ng h) ml(-1)), with an enantiomer ratio of 2.48. Copyright © 2012 Wiley Periodicals, Inc.

  10. A Novel and Rapid Method to Determine Doxycycline in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry

    PubMed Central

    Krishna, A. Chaitanya; Sathiyaraj, M.; Saravanan, R. S.; Chelladurai, R.; Vignesh, R.

    2012-01-01

    A simple, rapid, specific and sensitive liquid chromatography tandem mass spectrometric method has been developed and validated for the determination of doxycycline from the human plasma. Doxycycline is extracted from human plasma by solid phase extraction. Demeclocycline was used as an internal standard. Detection was performed at transitions of 444.800→428.200 for doxycycline and 464.700→448.100 for demeclocycline using mass spectrometry. Chromatographic separation of analyte and internal standard were carried out using a reverse phase C18, column at 0.500 ml/min flow. The assay of doxycycline is linear over the range of 0.055-7.612 μg/ml, with a precision <14.83%, regression coefficient (r2)=0.9961 and the limit of quantification in plasma for doxycycline was 0.055 μg/ml. Mean extraction recovery obtained was 95.55%. Samples are stable at room temperature for 6 h, processed samples were stable at least for 30.20 h and also stable at three freeze-thaw cycles. The method has been used to perform pharmacokinetic and bioequivalence studies in human plasma. PMID:23798780

  11. Dual loyalties and the ethical and human rights obligations of occupational health professionals.

    PubMed

    London, Leslie

    2005-04-01

    Underlying most ethical dilemmas in occupational health practice is the problem of Dual Loyalties where health professionals have simultaneous obligations, explicit or implicit, to a third party, usually a private employer. A literature review was undertaken of case studies of workplace occupational health conflicts, international human rights and ethical codes and strategies for managing dual loyalties, complemented by iterative discussions in an international working group convened to address the problem of Dual Loyalties. Violations of the worker-patient's human rights may arise from: (1) the incompatibility of simultaneous obligations; (2) pressure on the professional from the third party; and (3) separation of the health professional's clinical role from that of a social agent. The practitioner's contractual relationship with the third party is often the underlying problem, being far more explicit than their moral obligation to patients, and encouraging a social identification at the expense of a practitioner's professional identity. Because existing ethical guidelines lack specificity on managing Dual Loyalties in occupational health, guidelines that draw on human rights standards have been developed by the working group. These guidelines propose standards for individual professional conduct and complementary institutional mechanisms to address the problem. Copyright (c) 2005 Wiley-Liss, Inc.

  12. A validated HPLC determination of the flavone aglycone diosmetin in human plasma.

    PubMed

    Kanaze, Feras Imad; Bounartzi, Melpomeni I; Niopas, Ioannis

    2004-12-01

    Diosmetin, 3',5,7-trihydroxy-4'-methoxy flavone, is the aglycone of the flavonoid glycoside diosmin that occurs naturally in foods of plant origin. Diosmin exhibits antioxidant and anti-inflammatory activities, improves venous tone and it is used for the treatment of chronic venous insufficiency. Diosmin is hydrolyzed by enzymes of intestinal micro flora before absorption of its aglycone diosmetin. A specific, sensitive, precise, accurate and robust HPLC assay for the determination of diosmetin in human plasma was developed and validated. Diosmetin and the internal standard 7-ethoxycoumarin were isolated from plasma by liquid-liquid extraction and separated on a C8 reversed-phase column with methanol-water-acetic acid (55:43:2, v/v/v) as the mobile phase at 43 degrees C. Peaks were monitored at 344 nm. The method was linear in the 10-300 ng/mL concentration range (r > 0.999). Recovery for diosmetin and internal standard was greater than 89.7 and 86.8%, respectively. Intra-day and inter-day precision for diosmetin ranged from 1.6 to 4.6 and from 2.2 to 5.3%, respectively, and accuracy was better than 97.9%. Copyright 2004 John Wiley & Sons, Ltd.

  13. A rapid and sensitive LC-MS/MS-ESI method for the determination of tolvaptan and its two main metabolites in human plasma.

    PubMed

    Jiang, Juanjuan; Tian, Lei; Huang, Yiling; Yan, Yan; Li, Yishi

    2016-08-01

    A liquid chromatography-tandem mass spectrometry (LC-MS) method to quantify tolvaptan and its two main metabolites and applied to human study was first developed and validated as a measure of compliance in clinical research. Because of the structure similarity of tolvaptan and its multiple metabolites, the method was optimized to obtain a chromatographic and MS separation of the endogenous interference and isotope ions as well as high analysis throughput. Tolvaptan, its two main metabolites and the internal standard were extracted from human serum (0.1mL) using solid-phase extraction, separated on a Waters nova-pak C18 column (150×3.9mm, 5μm) using isocratic elution with a mobile phase composed of acetonitrile, water and formic acid (65:35:0.25, v/v/v). The total run-time was shortened to 3.5min. The mass transition ranges under positive electrospray ionisation that were monitored for quantitation included m/z 449-252 for tolvaptan, m/z 479-252 for metabolite DM-4103, m/z 481-252 for metabolite DM-4107 and m/z 463-266 for the internal standard (IS). The limit of quantification in plasma for all three analytes was 1ng/mL. The method was validated over a linear range from 1 to 500ng/mL for all three analytes with acceptable inter- and intra-assay precision and accuracy. The stability of the analytes was determined to be suitable for routine laboratory practices. The method was successfully applied to samples taken from research volunteers who ingested a 15mg tolvaptan tablet. Copyright © 2016. Published by Elsevier B.V.

  14. Liquid chromatography/tandem mass spectrometry method for simultaneous determination of cocaine and its metabolite (-)ecgonine methyl ester in human acidified stabilized plasma samples.

    PubMed

    Liu, Yongzhen; Zheng, Bo; Strafford, Stephanie; Orugunty, Ravi; Sullivan, Michael; Gus, Jeffrey; Heidbreder, Christian; Fudala, Paul J; Nasser, Azmi

    2014-06-15

    Two simple, sensitive and rapid liquid chromatography/electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) methods (low range and high range) were developed and validated for the quantification of cocaine and its metabolite (-)ecgonine methyl ester (EME) in human acidified stabilized plasma samples. In the low range assay, cocaine and the internal standard, cocaine-D3, were extracted using a single step liquid-liquid extraction from human acidified stabilized plasma. For the high range assay, human acidified stabilized plasma containing cocaine, EME, and the internal standards, cocaine-D3 and EME-D3, was mixed with acetonitrile, and the protein precipitate was separated by centrifugation. Both cocaine and EME extracted from both assays were separated on a HILIC column and detected in positive ion mode using multiple reaction monitoring (MRM). Both methods were validated and the specificity, linearity, lower limit of quantitation (LLOQ), precision, accuracy, recoveries and stability were determined. The linear range for the low range assay was 0.01-5ng/mL for cocaine; in the high range assay values were 5-1000ng/mL for cocaine and 1-200ng/mL for EME. The correlation coefficient (R(2)) values for both assays were 0.993 or greater. The precision and accuracy for intra-day and inter-day were better than 13.0%. The recovery was above 85% and matrix effects were low with the matrix factor ranging from 0.817 to 1.10 for both analytes in both assays. The validated methods were successfully used to quantify the plasma concentrations of cocaine and EME in clinical pharmacokinetic and pharmacodynamic studies. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. 77 FR 37361 - National Emission Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-06-21

    ... National Emission Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion Engines; New Source Performance Standards for Stationary Internal Combustion Engines AGENCY: Environmental Protection... Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion Engines; New Source Performance...

  16. 78 FR 63873 - Minimum Internal Control Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-10-25

    ... Internal Control Standards AGENCY: National Indian Gaming Commission, Interior. ACTION: Final rule. SUMMARY: The National Indian Gaming Commission (NIGC) amends its minimum internal control standards for Class... Internal Control Standards. 64 FR 590. The rule added a new part to the Commission's regulations...

  17. 78 FR 11793 - Minimum Internal Control Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-02-20

    ... Internal Control Standards AGENCY: National Indian Gaming Commission. ACTION: Proposed rule. SUMMARY: The National Indian Gaming Commission (NIGC) proposes to amend its minimum internal control standards for Class... NIGC published a final rule in the Federal Register called Minimum Internal Control Standards. 64 FR...

  18. 47 CFR 76.612 - Cable television frequency separation standards.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 47 Telecommunication 4 2011-10-01 2011-10-01 false Cable television frequency separation standards. 76.612 Section 76.612 Telecommunication FEDERAL COMMUNICATIONS COMMISSION (CONTINUED) BROADCAST RADIO SERVICES MULTICHANNEL VIDEO AND CABLE TELEVISION SERVICE Technical Standards § 76.612 Cable television...

  19. Australia and international treaties: population.

    PubMed

    Hugo, G

    1995-05-01

    "The separation of environmental and population issues globally is reflected in the fact that the setting of international agendas to tackle them was for all intents and purposes undertaken at separate international meetings--the Earth Summit in Rio de Janeiro in 1992 and the International Population Conference in Cairo in 1994. This paper presents an overview of Australia's international involvement in population issues and suggests that until recently Australia had played a minor political role in international population initiatives primarily, and perhaps ironically, because it has been a world leader in demographic research and teaching for several decades." excerpt

  20. 77 FR 32444 - Minimum Internal Control Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-06-01

    ... Internal Control Standards AGENCY: National Indian Gaming Commission. ACTION: Proposed rule. SUMMARY: The National Indian Gaming Commission (NIGC) proposes to amend its minimum internal control standards for Class... the Federal Register called Minimum Internal Control Standards. 64 FR 590. The rule added a new part...

  1. Micellar electrokinetic capillary chromatographic method for the quantitative analysis of uricosuric and antigout drugs in pharmaceutical preparations.

    PubMed

    Kou, Hwang-Shang; Lin, Tsai-Pei; Chung, Tang-Chia; Wu, Hsin-Lung

    2006-06-01

    A simple MEKC method is described for the separation and quantification of seven widely used uricosuric and antigout drugs, including allopurinol (AP), benzbromarone (BZB), colchicine (COL), orotic acid (OA), oxypurinol (OP), probenecid (PB), and sulfinpyrazone (SPZ). The drugs were separated in a BGE of borate buffer (45 mM; pH 9.00) with SDS (20 mM) as the micellar source and the separated drugs were directly monitored with a UV detector (214 nm). Several parameters affecting the separation and analysis of the drugs were studied. Based on the normalized peak-area ratios of the drugs to an internal standard versus the concentration of the drugs, the method is applicable to quantify BZB, COL, and SPZ (each 5-200 microM), AP, OA, OP, and PB (each 10-200 microM) with detection limits (S/N = 3, 0.5 psi, 5 s injection) in the range of 0.6-4.0 microM. The precision (RSD; n = 5) and accuracy (relative error; n = 5) of the method for intraday and interday analyses of the analytes at three levels (30, 120, and 180 microM) are below 4% (n = 3). The method was demonstrated to be suitable for the analysis of AP and COL in commercial tablets with speed and simplicity.

  2. Determination of hydroxyurea in human plasma by HPLC-UV using derivatization with xanthydrol.

    PubMed

    Legrand, Tiphaine; Rakotoson, Marie-Georgine; Galactéros, Frédéric; Bartolucci, Pablo; Hulin, Anne

    2017-10-01

    A simple and rapid high performance liquid chromatography (HPLC) method using ultraviolet (UV) detection was developed to determine hydroxyurea (HU) concentration in plasma sample after derivatization with xanthydrol. Two hundred microliters samples were spiked with methylurea (MeU) as internal standard and proteins were precipitated by adding methanol. Derivatization of HU and MeU was immediately performed by adding 0.02M xanthydrol and 1.5M HCl in order to obtain xanthyl-derivatives of HU and MeU that can be further separated using HPLC and quantified using UV detection at 240nm. Separation was achieved using a C18 column with a mobile phase composed of 20mM ammonium acetate and acetonitrile in gradient elution mode at a flow rate of 1mL/min. The total analysis time did not exceed 18min. The method was found linear from 5 to 400μM and all validation parameters fulfilled the international requirements. Between- and within-run accuracy error ranged from -4.7% to 3.2% and precision was lower than 12.8%. This simple method requires small volume samples and can be easily implemented in most clinical laboratories to develop pharmacokinetics studies of HU and to promote its therapeutic monitoring. Copyright © 2017 Elsevier B.V. All rights reserved.

  3. Silicosis in Workers Exposed to Artificial Quartz Conglomerates: Does It Differ From Chronic Simple Silicosis?

    PubMed

    Paolucci, Valentina; Romeo, Riccardo; Sisinni, Antonietta Gerardina; Bartoli, Dusca; Mazzei, Maria Antonietta; Sartorelli, Pietro

    2015-12-01

    Recently, a number of reports have been published on silicosis in workers exposed to artificial quartz conglomerates containing high levels of crystalline silica particles (70-90%) used in the construction of kitchen and bathroom surfaces. Three cases of silicosis in workers exposed to artificial quartz conglomerates are reported. The diagnosis was derived from both the International Labour Office and the International Classification of HRCT for Occupational and Environmental Respiratory Diseases (ICOERD) classifications and cytological analysis of bronchoalveolar lavage fluid. In 2 cases, levels of respirable silica greatly in excess of recommended standards were measured in the workplace, and cytological analysis of bronchoalveolar lavage fluid highlighted a prevalence of lymphocytes, meeting criteria for the diagnosis of accelerated silicosis. The prevention of pneumoconiosis caused by the use of innovative materials, such as artificial conglomerates with high crystalline silica content must be addressed. Copyright © 2014 SEPAR. Published by Elsevier Espana. All rights reserved.

  4. Defining the clinical course of multiple sclerosis

    PubMed Central

    Reingold, Stephen C.; Cohen, Jeffrey A.; Cutter, Gary R.; Sørensen, Per Soelberg; Thompson, Alan J.; Wolinsky, Jerry S.; Balcer, Laura J.; Banwell, Brenda; Barkhof, Frederik; Bebo, Bruce; Calabresi, Peter A.; Clanet, Michel; Comi, Giancarlo; Fox, Robert J.; Freedman, Mark S.; Goodman, Andrew D.; Inglese, Matilde; Kappos, Ludwig; Kieseier, Bernd C.; Lincoln, John A.; Lubetzki, Catherine; Miller, Aaron E.; Montalban, Xavier; O'Connor, Paul W.; Petkau, John; Pozzilli, Carlo; Rudick, Richard A.; Sormani, Maria Pia; Stüve, Olaf; Waubant, Emmanuelle; Polman, Chris H.

    2014-01-01

    Accurate clinical course descriptions (phenotypes) of multiple sclerosis (MS) are important for communication, prognostication, design and recruitment of clinical trials, and treatment decision-making. Standardized descriptions published in 1996 based on a survey of international MS experts provided purely clinical phenotypes based on data and consensus at that time, but imaging and biological correlates were lacking. Increased understanding of MS and its pathology, coupled with general concern that the original descriptors may not adequately reflect more recently identified clinical aspects of the disease, prompted a re-examination of MS disease phenotypes by the International Advisory Committee on Clinical Trials of MS. While imaging and biological markers that might provide objective criteria for separating clinical phenotypes are lacking, we propose refined descriptors that include consideration of disease activity (based on clinical relapse rate and imaging findings) and disease progression. Strategies for future research to better define phenotypes are also outlined. PMID:24871874

  5. Liquid helium cryostat with internal fluorescence detection for x-ray absorption studies in the 2-6 keV energy region

    NASA Astrophysics Data System (ADS)

    McFarlane Holman, Karen L.; Latimer, Matthew J.; Yachandra, Vittal K.

    2004-06-01

    X-ray absorption spectroscopy (XAS) in the intermediate x-ray region (2-6 keV) for dilute biological samples has been limited because of detector/flux limitations and inadequate cryogenic instrumentation. We have designed and constructed a new tailpiece/sample chamber for a commercially available liquid helium cooled cryostat which overcomes difficulties related to low fluorescence signals by using thin window materials and incorporating an internal photodiode detector. With the apparatus, XAS data at the Cl, S, and Ca K edges have been collected on frozen solutions and biological samples at temperatures down to 60 K. A separate chamber has been incorporated for collecting room-temperature spectra of standard compounds (for energy calibration purposes) which prevents contamination of the cryostat chamber and allows the sample to remain undisturbed, both important concerns for studying dilute and radiation-sensitive samples.

  6. Significant Improvements in the Practice Patterns of Adult Related Donor Care in US Transplantation Centers.

    PubMed

    Anthias, Chloe; Shaw, Bronwen E; Kiefer, Deidre M; Liesveld, Jane L; Yared, Jean; Kamble, Rammurti T; D'Souza, Anita; Hematti, Peiman; Seftel, Matthew D; Norkin, Maxim; DeFilipp, Zachariah; Kasow, Kimberly A; Abidi, Muneer H; Savani, Bipin N; Shah, Nirali N; Anderlini, Paolo; Diaz, Miguel A; Malone, Adriana K; Halter, Joerg P; Lazarus, Hillard M; Logan, Brent R; Switzer, Galen E; Pulsipher, Michael A; Confer, Dennis L; O'Donnell, Paul V

    2016-03-01

    Recent investigations have found a higher incidence of adverse events associated with hematopoietic cell donation in related donors (RDs) who have morbidities that if present in an unrelated donor (UD) would preclude donation. In the UD setting, regulatory standards ensure independent assessment of donors, one of several crucial measures to safeguard donor health and safety. A survey conducted by the Center for International Blood and Marrow Transplant Research (CIBMTR) Donor Health and Safety Working Committee in 2007 reported a potential conflict of interest in >70% of US centers, where physicians had simultaneous responsibility for RDs and their recipients. Consequently, several international organizations have endeavored to improve practice through regulations and consensus recommendations. We hypothesized that the changes in the 2012 Foundation for the Accreditation of Cellular Therapy and the Joint Accreditation Committee-International Society for Cellular Therapy and European Society for Blood and Marrow Transplantation standards resulting from the CIBMTR study would have significantly impacted practice. Accordingly, we conducted a follow-up survey of US transplantation centers to assess practice changes since 2007, and to investigate additional areas where RD care was predicted to differ from UD care. A total of 73 centers (53%), performing 79% of RD transplantations in the United States, responded. Significant improvements were observed since the earlier survey; 62% centers now ensure separation of RD and recipient care (P < .0001). This study identifies several areas where RD management does not meet international donor care standards, however. Particular concerns include counseling and assessment of donors before HLA typing, with 61% centers first disclosing donor HLA results to an individual other than the donor, the use of unlicensed mobilization agents, and the absence of long-term donor follow-up. Recommendations for improvement are made. Copyright © 2016 American Society for Blood and Marrow Transplantation. Published by Elsevier Inc. All rights reserved.

  7. Standards for UNiversal reporting of patient Decision Aid Evaluation studies: the development of SUNDAE Checklist.

    PubMed

    Sepucha, Karen R; Abhyankar, Purva; Hoffman, Aubri S; Bekker, Hilary L; LeBlanc, Annie; Levin, Carrie A; Ropka, Mary; Shaffer, Victoria A; Sheridan, Stacey L; Stacey, Dawn; Stalmeier, Peep; Vo, Ha; Wills, Celia E; Thomson, Richard

    2018-05-01

    Patient decision aids (PDAs) are evidence-based tools designed to help patients make specific and deliberated choices among healthcare options. The International Patient Decision Aid Standards (IPDAS) Collaboration review papers and Cochrane systematic review of PDAs have found significant gaps in the reporting of evaluations of PDAs, including poor or limited reporting of PDA content, development methods and delivery. This study sought to develop and reach consensus on reporting guidelines to improve the quality of publications evaluating PDAs. An international workgroup, consisting of members from IPDAS Collaboration, followed established methods to develop reporting guidelines for PDA evaluation studies. This paper describes the results from three completed phases: (1) planning, (2) drafting and (3) consensus, which included a modified, two-stage, online international Delphi process. The work was conducted over 2 years with bimonthly conference calls and three in-person meetings. The workgroup used input from these phases to produce a final set of recommended items in the form of a checklist. The SUNDAE Checklist (Standards for UNiversal reporting of patient Decision Aid Evaluations) includes 26 items recommended for studies reporting evaluations of PDAs. In the two-stage Delphi process, 117/143 (82%) experts from 14 countries completed round 1 and 96/117 (82%) completed round 2. Respondents reached a high level of consensus on the importance of the items and indicated strong willingness to use the items when reporting PDA studies. The SUNDAE Checklist will help ensure that reports of PDA evaluation studies are understandable, transparent and of high quality. A separate Explanation and Elaboration publication provides additional details to support use of the checklist. © 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.

  8. The Third International Standard for Corticotrophin

    PubMed Central

    Bangham, D. R.; Mussett, M. V.; Stack-Dunne, M. P.

    1962-01-01

    At its meeting in September 1957, the WHO Expert Committee on Biological Standardization agreed with the recommendation of the International Conference on Corticotrophin, held in July 1957, that a new international standard for corticotrophin should be set up, since the Second International Standard was made from crude material and was unsuitable for the assay of the purer preparations of corticotrophin now in general clinical use. In this paper, the authors describe the steps taken to establish the Third International Standard for Corticotrophin, from the preparation and international collaborative assay of the new material to the choice of the ”subcutaneous assay” for deriving the potency. The clinical and pharmacological implications of this choice are discussed. Since the preparation, characterization and exact quantitative assay of standards for corticotrophin are so difficult, several batches of approximately 3500 ampoules were prepared in a similar way from the same material to serve as an international Working Standard. Samples from two batches were included in the collaborative assay and found to have the same potency as the Third Standard. Sufficient ampoules of the Working Standard are available for use as national and laboratory standards. PMID:13966359

  9. Nontargeted quantitation of lipid classes using hydrophilic interaction liquid chromatography-electrospray ionization mass spectrometry with single internal standard and response factor approach.

    PubMed

    Cífková, Eva; Holčapek, Michal; Lísa, Miroslav; Ovčačíková, Magdaléna; Lyčka, Antonín; Lynen, Frédéric; Sandra, Pat

    2012-11-20

    The identification and quantitation of a wide range of lipids in complex biological samples is an essential requirement for the lipidomic studies. High-performance liquid chromatography-mass spectrometry (HPLC/MS) has the highest potential to obtain detailed information on the whole lipidome, but the reliable quantitation of multiple lipid classes is still a challenging task. In this work, we describe a new method for the nontargeted quantitation of polar lipid classes separated by hydrophilic interaction liquid chromatography (HILIC) followed by positive-ion electrospray ionization mass spectrometry (ESI-MS) using a single internal lipid standard to which all class specific response factors (RFs) are related to. The developed method enables the nontargeted quantitation of lipid classes and molecules inside these classes in contrast to the conventional targeted quantitation, which is based on predefined selected reaction monitoring (SRM) transitions for selected lipids only. In the nontargeted quantitation method described here, concentrations of lipid classes are obtained by the peak integration in HILIC chromatograms multiplied by their RFs related to the single internal standard (i.e., sphingosyl PE, d17:1/12:0) used as common reference for all polar lipid classes. The accuracy, reproducibility and robustness of the method have been checked by various means: (1) the comparison with conventional lipidomic quantitation using SRM scans on a triple quadrupole (QqQ) mass analyzer, (2) (31)P nuclear magnetic resonance (NMR) quantitation of the total lipid extract, (3) method robustness test using subsequent measurements by three different persons, (4) method transfer to different HPLC/MS systems using different chromatographic conditions, and (5) comparison with previously published results for identical samples, especially human reference plasma from the National Institute of Standards and Technology (NIST human plasma). Results on human plasma, egg yolk and porcine liver extracts are presented and discussed.

  10. Validation of a method for the determination of zolpidem in human plasma using LC with fluorescence detection.

    PubMed

    Ring, P R; Bostick, J M

    2000-04-01

    A sensitive and selective high-performance liquid chromatography (HPLC) method was developed for the determination of zolpidem in human plasma. Zolpidem and the internal standard (trazodone) were extracted from human plasma that had been made basic. The basic sample was loaded onto a conditioned Bond Elut C18 cartridge, rinsed with water and eluted with methanol. Forty microliters were then injected onto the LC system. Separation was achieved on a C18 column (150 x 4.6 mm, 5 microm) with a mobile phase composed of acetonitrile:50 mM potassium phosphate monobasic at pH 6.0 (4:6, v/v). Detection was by fluorescence, with excitation at 254 nm and emission at 400 nm. The retention times of zolpidem and internal standard were approximately 4.7 and 5.3 min, respectively. The LC run time was 8 min. The assay was linear in concentration range 1-400 ng/ml for zolpidem in human plasma. The analysis of quality control samples for zolpidem (3, 30, and 300 ng/ml) demonstrated excellent precision with relative standard deviations (RSD) of 3.7, 4.6, and 3.0%, respectively (n = 18). The method was accurate with all intraday (n = 6) and overall (n = 18) mean concentrations within 5.8% from nominal at all quality control sample concentrations. This method was also performed using a Gilson Aspec XL automated sample processor and autoinjector. The samples were manually fortified with internal standard and made basic. The aspec then performed the solid phase extraction and made injections of the samples onto the LC system. Using the automated procedure for analysis, quality control samples for zolpidem (3, 30, and 300 ng/ml) demonstrated acceptable precision with RSD values of 9.0, 4.9, and 5.1%, respectively (n = 12). The method was accurate with all intracurve (n = 4) and overall (n = 12) mean values being less than 10.8% from nominal at all quality control sample concentrations.

  11. 78 FR 21060 - Appeal Proceedings Before the Commission

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-04-09

    ... adoption of alternate standards from those required by the Commission's minimum internal control standards... adoption of alternate standards from those required by the Commission's minimum internal control standards... TGRAs' adoption of alternate standards from those required by the Commission's minimum internal control...

  12. 40 CFR 60.692-3 - Standards: Oil-water separators.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... Emissions From Petroleum Refinery Wastewater Systems § 60.692-3 Standards: Oil-water separators. (a) Each... wastewater shall, in addition to the requirements in paragraph (a) of this section, be equipped and operated... wastewater which was equipped and operated with a fixed roof covering the entire separator tank or a portion...

  13. 40 CFR 60.692-3 - Standards: Oil-water separators.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Emissions From Petroleum Refinery Wastewater Systems § 60.692-3 Standards: Oil-water separators. (a) Each... wastewater shall, in addition to the requirements in paragraph (a) of this section, be equipped and operated... wastewater which was equipped and operated with a fixed roof covering the entire separator tank or a portion...

  14. Multiple fuel supply system for an internal combustion engine

    DOEpatents

    Crothers, William T.

    1977-01-01

    A multiple fuel supply or an internal combustion engine wherein phase separation of components is deliberately induced. The resulting separation permits the use of a single fuel tank to supply components of either or both phases to the engine. Specifically, phase separation of a gasoline/methanol blend is induced by the addition of a minor amount of water sufficient to guarantee separation into an upper gasoline phase and a lower methanol/water phase. A single fuel tank holds the two-phase liquid with separate fuel pickups and separate level indicators for each phase. Either gasoline or methanol, or both, can be supplied to the engine as required by predetermined parameters. A fuel supply system for a phase-separated multiple fuel supply contained in a single fuel tank is described.

  15. A new standardized method for quantification of humic and fulvic acids in humic ores and commercial products.

    PubMed

    Lamar, Richard T; Olk, Daniel C; Mayhew, Lawrence; Bloom, Paul R

    2014-01-01

    Increased use of humic substances in agriculture has generated intense interest among producers, consumers, and regulators for an accurate and reliable method to quantify humic acid (HA) and fulvic acid (FA) in raw ores and products. Here we present a thoroughly validated method, the new standardized method for determination of HA and FA contents in raw humate ores and in solid and liquid products produced from them. The methods used for preparation of HA and FA were adapted according to the guidelines of the International Humic Substances Society involving alkaline extraction followed by acidification to separate HA from the fulvic fraction. This is followed by separation of FA from the fulvic fraction by adsorption on a nonionic macroporous acrylic ester resin at acid pH. It differs from previous methods in that it determines HA and FA concentrations gravimetrically on an ash-free basis. Critical steps in the method, e.g., initial test portion mass, test portion to extract volume ratio, extraction time, and acidification of alkaline extract, were optimized for maximum and consistent recovery of HA and FA. The method detection limits for HA and FA were 4.62 and 4.8 mg/L, respectively. The method quantitation limits for HA and FA were 14.7 and 15.3 mg/L, respectively.

  16. New separators for nickel-zinc batteries

    NASA Technical Reports Server (NTRS)

    Sheibley, D. W.

    1976-01-01

    Flexible separators consisting of a substrate coated with a mixture of a polymer and organic and inorganic additives were cycle tested in nickel-zinc cells. By substituting a rubber-based resin for polyphenylene oxide in the standard inorganic-organic separator, major improvements in both cell life and flexibility were made. Substituting newsprint for asbestos as the substrate shows promise for use on the zinc electrode and reduces separator cost. The importance of ample electrolyte in the cells was noted. Cycle lives and the characteristics of these flexible, low-cost separators were compared with those of a standard microporous polypropylene separator.

  17. High-speed liquid chromatographic determination of pilocarpine in pharmaceutical dosage forms.

    PubMed

    Khalil, S K

    1977-11-01

    A specific method for the direct determination of pilocarpine in aqueous pharmaceuticals in the presence of decomposition products, methylcellulose, and other ingredients usually present in pharmaceuticals is described. The method involves separation by high-speed liquid chromatography using, in series, octadecylsilane bonded to silica and cyanopropylsilane bonded to silica columns and a tetrahydrofuran-pH 9.2 borate buffer (3:7) eluant. Quantitation is achieved by monitoring the absorbance of the effluent at 254 nm and using a pyridine internal standard and a calibration curve prepared from known concentrations of pilocarpine nitrate. The reproducibility of the retention time and peak area was better than 2.0%.

  18. Simultaneous analysis of tea catechins, caffeine, gallic acid, theanine and ascorbic acid by micellar electrokinetic capillary chromatography.

    PubMed

    Aucamp, J P; Hara, Y; Apostolides, Z

    2000-04-21

    A micellar electrokinetic capillary chromatography (MEKC) method for the simultaneous analysis of five tea catechins, theanine, caffeine, gallic acid and ascorbic acid has been developed. The catechins are (-)-epicatechin, (+)-catechin, (-)-epigallocatechin, (-)-epicatechin gallate and (-)-epigallocatechin gallate. p-Nitrophenol serves as both reference and internal standard. All the components are separated within 13 min with a 57 cm uncoated fused-silica column. On-column detection was carried out at 200 nm. This method has been used to measure these compounds in fresh tea leaves and tea liquor. The limit of detection for all analytes ranged from 1 to 20 microg/ml.

  19. 7 CFR 801.4 - Tolerances for dockage testers.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ....10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Riddle separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Sieve separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Total...

  20. 7 CFR 801.4 - Tolerances for dockage testers.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ....10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Riddle separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Sieve separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Total...

  1. 7 CFR 801.4 - Tolerances for dockage testers.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ....10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Riddle separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Sieve separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Total...

  2. 7 CFR 801.4 - Tolerances for dockage testers.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ....10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Riddle separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Sieve separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Total...

  3. 7 CFR 801.4 - Tolerances for dockage testers.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ....10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Riddle separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Sieve separation ±0.10 percent, mean deviation from standard dockage tester using Hard Red Winter wheat Total...

  4. Determination of emamectin benzoate in medicated fish feed.

    PubMed

    Farer, L J; Hayes, J; Rosen, J; Knight, P

    1999-01-01

    A method was developed to quantitate emamectin benzoate in fish feed at levels between 5 and 15 ppm. The active ingredient is extracted from 20 g medicated feed into aqueous-methanolic solvent by overnight shaking. A solid-phase extraction procedure using a 2 g C18 cartridge is then used to concentrate the active residue and remove interfering matrix components. The extracted drug and internal standard are eluted from the cartridge, evaporated to dryness, and reconstituted in methanol. A control feed sample and fortified control working standard are simultaneously prepared. Remaining interferences and sample analysis are further separated on a gradient liquid chromatographic system. Recovery of emamectin benzoate from fortified feeds ranged from 97 to 100%, with a coefficient of variation (CV) of 1.2%. Determination of emamectin benzoate in medicated feeds resulted in CVs ranging from 2.3 to 4.2% and recoveries of 88 to 98% of label claim.

  5. Determination of gamma-aminobutyric acid in food matrices by isotope dilution hydrophilic interaction chromatography coupled to mass spectrometry.

    PubMed

    Zazzeroni, Raniero; Homan, Andrew; Thain, Emma

    2009-08-01

    The estimation of the dietary intake of gamma-aminobutyric acid (GABA) is dependent upon the knowledge of its concentration values in food matrices. To this end, an isotope dilution liquid chromatography-mass spectrometry method has been developed employing the hydrophilic interaction chromatography technique for analyte separation. This approach enabled accurate quantification of GABA in apple, potato, soybeans, and orange juice without the need of a pre- or post-column derivatization reaction. A selective and precise analytical measurement has been obtained with a triple quadrupole mass spectrometer operating in multiple reaction monitoring using the method of standard additions and GABA-d(6) as an internal standard. The concentrations of GABA found in the matrices tested are 7 microg/g of apple, 342 microg/g of potatoes, 211 microg/g of soybeans, and 344 microg/mL of orange juice.

  6. Wake Vortex Advisory System (WakeVAS) Concept of Operations

    NASA Technical Reports Server (NTRS)

    Rutishauser, David; Lohr, Gary; Hamilton, David; Powers, Robert; McKissick, Burnell; Adams, Catherine; Norris, Edward

    2003-01-01

    NASA Langley Research Center has a long history of aircraft wake vortex research, with the most recent accomplishment of demonstrating the Aircraft VOrtex Spacing System (AVOSS) at Dallas/Forth Worth International Airport in July 2000. The AVOSS was a concept for an integration of technologies applied to providing dynamic wake-safe reduced spacing for single runway arrivals, as compared to current separation standards applied during instrument approaches. AVOSS included state-of-the-art weather sensors, wake sensors, and a wake behavior prediction algorithm. Using real-time data AVOSS averaged a 6% potential throughput increase over current standards. This report describes a Concept of Operations for applying the technologies demonstrated in the AVOSS to a variety of terminal operations to mitigate wake vortex capacity constraints. A discussion of the technological issues and open research questions that must be addressed to design a Wake Vortex Advisory System (WakeVAS) is included.

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

    PubMed

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

    2005-01-01

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

  8. Using FTIR-ATR Spectroscopy to Teach the Internal Standard Method

    ERIC Educational Resources Information Center

    Bellamy, Michael K.

    2010-01-01

    The internal standard method is widely applied in quantitative analyses. However, most analytical chemistry textbooks either omit this topic or only provide examples of a single-point internal standardization. An experiment designed to teach students how to prepare an internal standard calibration curve is described. The experiment is a modified…

  9. To recognize the use of international standards for making harmonized regulation of medical devices in Asia-pacific.

    PubMed

    Anand, K; Saini, Ks; Chopra, Y; Binod, Sk

    2010-07-01

    'Medical Devices' include everything from highly sophisticated, computerized, medical equipment, right down to simple wooden tongue depressors. Regulations embody the public expectations for how buildings and facilities are expected to perform and as such represent public policy. Regulators, who develop and enforce regulations, are empowered to act in the public's interest to set this policy and are ultimately responsible to the public in this regard. Standardization contributes to the basic infrastructure that underpins society including health and environment, while promoting sustainability and good regulatory practice. The international organizations that produce International Standards are the International Electrotechnical Commission (IEC), the International Organization for Standardization (ISO), and the International Telecommunication Union (ITU). With the increasing globalization of markets, International Standards (as opposed to regional or national standards) have become critical to the trading process, ensuring a level playing field for exports, and ensuring that imports meet the internationally recognized levels of performance and safety. The development of standards is done in response to sectors and stakeholders that express a clearly established need for them. An industry sector or other stakeholder group typically communicates its requirement for standards to one of the national members. To be accepted for development, a proposed work item must receive a majority support of the participating members, who verify the global relevance of the proposed item. The regulatory authority (RA) should provide a method for the recognition of international voluntary standards and for public notification of such recognition. The process of recognition may vary from country to country. Recognition may occur by periodic publication of lists of standards that a regulatory authority has found will meet the Essential Principles. In conclusion, International standards, such as, basic standards, group standards, and product standards, are a tool for harmonizing regulatory processes, to assure the safety, quality, and performance of medical devices. Standards represent the opinion of experts from all interested parties, including industry, regulators, users, and others.

  10. 78 FR 18321 - International Code Council: The Update Process for the International Codes and Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-03-26

    ... for Residential Construction in High Wind Regions. ICC 700: National Green Building Standard The..., coordinated, and necessary to regulate the built environment. Federal agencies frequently use these codes and... International Codes and Standards consist of the following: ICC Codes International Building Code. International...

  11. Fifth International Standard for Gas-Gangrene Antitoxin (Perfringens) (Clostridium welchii Type A Antitoxin)

    PubMed Central

    Evans, D. G.; Perkins, F. T.

    1963-01-01

    The Fifth International Standard Gas-Gangrene Antitoxin (Perfringens) (Clostridium welchii Type A Antitoxin) was prepared from serum from immunized horses. It was freeze-dried in ampoules each containing 1 ml. Seven laboratories collaborated in assaying its potency in terms of the Fourth International Standard by the intravenous inoculation of mice. The geometric mean value, taking the results of all the laboratories, was 270 International Units per ampoule and the maximum variation between laboratories was 15%. In vitro (lecithinase) tests were also done by three laboratories, giving an average of 261 International Units per ampoule. The dry weight contents of ampoules, determined in three laboratories, varied by less than 3%, with an average of 90.35 mg per ampoule. The standard was stable for 120 hours at 56°C. Each ampoule of the Fifth International Standard for Gas-Gangrene Antitoxin (Perfringens) contains 270 International Units, and one International Unit is contained in 0.3346 mg of the International Standard. PMID:14107745

  12. Three-dimensional analysis of magnetometer array data

    NASA Technical Reports Server (NTRS)

    Richmond, A. D.; Baumjohann, W.

    1984-01-01

    A technique is developed for mapping magnetic variation fields in three dimensions using data from an array of magnetometers, based on the theory of optimal linear estimation. The technique is applied to data from the Scandinavian Magnetometer Array. Estimates of the spatial power spectra for the internal and external magnetic variations are derived, which in turn provide estimates of the spatial autocorrelation functions of the three magnetic variation components. Statistical errors involved in mapping the external and internal fields are quantified and displayed over the mapping region. Examples of field mapping and of separation into external and internal components are presented. A comparison between the three-dimensional field separation and a two-dimensional separation from a single chain of stations shows that significant differences can arise in the inferred internal component.

  13. The second international standard for polymyxin B.

    PubMed

    Lightbown, J W; Thomas, A H; Grab, B; Outschoorn, A S

    1973-01-01

    Since supplies of the first International Standard for Polymyxin B were exhausted, it was replaced by a second international standard the potency of which was estimated from the results of a collaborative assay carried out by 5 laboratories in 4 countries. The wide variations in the results probably resulted from difficulties experienced in handling the first international standard. The potency finally agreed upon by the collaborating laboratories, on the basis of the overall mean values obtained after rejection of the most discrepant assays, was 8 403 IU/mg. That value was accepted by the WHO Expert Committee on Biological Standardization (1970), which consequently defined the International Unit of polymyxin B as the activity contained in 0.000119 mg of the second international standard.

  14. The second international standard for polymyxin B*

    PubMed Central

    Lightbown, J. W.; Thomas, A. H.; Grab, B.; Outschoorn, A. S.

    1973-01-01

    Since supplies of the first International Standard for Polymyxin B were exhausted, it was replaced by a second international standard the potency of which was estimated from the results of a collaborative assay carried out by 5 laboratories in 4 countries. The wide variations in the results probably resulted from difficulties experienced in handling the first international standard. The potency finally agreed upon by the collaborating laboratories, on the basis of the overall mean values obtained after rejection of the most discrepant assays, was 8 403 IU/mg. That value was accepted by the WHO Expert Committee on Biological Standardization (1970), which consequently defined the International Unit of polymyxin B as the activity contained in 0.000119 mg of the second international standard. PMID:4350877

  15. Standardized sign-out reduces intern perception of medical errors on the general internal medicine ward.

    PubMed

    Salerno, Stephen M; Arnett, Michael V; Domanski, Jeremy P

    2009-01-01

    Prior research on reducing variation in housestaff handoff procedures have depended on proprietary checkout software. Use of low-technology standardization techniques has not been widely studied. We wished to determine if standardizing the process of intern sign-out using low-technology sign-out tools could reduce perception of errors and missing handoff data. We conducted a pre-post prospective study of a cohort of 34 interns on a general internal medicine ward. Night interns coming off duty and day interns reassuming care were surveyed on their perception of erroneous sign-out data, mistakes made by the night intern overnight, and occurrences unanticipated by sign-out. Trainee satisfaction with the sign-out process was assessed with a 5-point Likert survey. There were 399 intern surveys performed 8 weeks before and 6 weeks after the introduction of a standardized sign-out form. The response rate was 95% for the night interns and 70% for the interns reassuming care in the morning. After the standardized form was introduced, night interns were significantly (p < .003) less likely to detect missing sign-out data including missing important diseases, contingency plans, or medications. Standardized sign-out did not significantly alter the frequency of dropped tasks or missed lab and X-ray data as perceived by the night intern. However, the day teams thought there were significantly less perceived errors on the part of the night intern (p = .001) after introduction of the standardized sign-out sheet. There was no difference in mean Likert scores of resident satisfaction with sign-out before and after the intervention. Standardized written sign-out sheets significantly improve the completeness and effectiveness of handoffs between night and day interns. Further research is needed to determine if these process improvements are related to better patient outcomes.

  16. Association of two single-isomer anionic CD in NACE for the chiral and achiral separation of fenbendazole, its sulphoxide and sulphone metabolites: application to their determination after in vitro metabolism.

    PubMed

    Rousseau, Anne; Gillotin, Florian; Chiap, Patrice; Crommen, Jacques; Fillet, Marianne; Servais, Anne-Catherine

    2010-05-01

    A NACE method was developed for the separation of fenbendazole (FBZ), a prochiral drug giving rise to chiral (oxfendazole or OFZ) and nonchiral (FBZ sulphone or FBZSO(2)) metabolites. First, the effect of the nature and the concentration of CD as well as that of the acidic BGE on the enantiomeric separation of OFZ were studied. OFZ enantiomers were completely resolved using a BGE made up of 10 mM ammonium formate and 0.5 M TFA in methanol containing 10 mM heptakis(2,3-di-O-acetyl-6-O-sulfo)-beta-CD and 10 mM heptakis(2,3-di-O-methyl-6-O-sulfo)-beta-CD. Moreover, the NACE method was found to be particularly well suited to the simultaneous determination of FBZ, OFZ enantiomers, and FBZSO(2). Thiabendazole was selected as an internal standard. The CD-NACE potential was then evaluated for in vitro metabolism studies using FBZ as a model case. The OFZ enantiomers and FBZSO(2) could be detected after incubation of FBZ in the phenobarbital-induced male rat liver microsomes systems.

  17. Preparative Separation and Purification of the Total Flavonoids in Scorzonera austriaca with Macroporous Resins.

    PubMed

    Xie, Yang; Guo, Qiu-Shi; Wang, Guang-Shu

    2016-06-13

    The use of macroporous resins for the separation and purification of total flavonoids to obtain high-purity total flavonoids from Scorzonera austriaca was studied. The optimal conditions for separation and purification of total flavonoids in S. austriaca with macroporous resins were as follows: D4020 resin columns were loaded with crude flavonoid extract solution, and after reaching adsorptive saturation, the columns were eluted successively with 5 bed volumes (BV) of water, 5 BV of 5% (v/v) aqueous ethanol and 5 BV of 30% (v/v) aqueous ethanol at an elute flow rate of 2 BV·h(-1). Total flavonoids were obtained from the 30% aqueous ethanol eluate by vacuum distillation recovery. The content of flavonoid compounds in the total flavonoids was 93.5%, which represents an improvement by about 150%. In addition, five flavonoid compounds in the product were identified as 2″-O-β-d-xylopyranosyl isoorientin, 6-C-α-l-arabipyranosyl orientin, orientin, isoorientin and vitexin by LC-ESI-MS analysis and internal standard methods. The results in this study could represent a method for the large-scale production of total flavonoids from S. austriaca.

  18. Tongue's substance and coating recognition analysis using HSV color threshold in tongue diagnosis

    NASA Astrophysics Data System (ADS)

    Kamarudin, Nur Diyana; Ooi, Chia Yee; Kawanabe, Tadaaki; Mi, Xiaoyu

    2016-07-01

    In ISO TC249 conference, tongue diagnosis has been one of the most active research and their objectifications has become significant with the help of numerous statistical and machine learning algorithm. Color information of substance or tongue body has kept valuable information regarding the state of disease and its correlation with the internal organs. In order to produce high reproducibility of color measurement analysis, tongue images have to undergo several procedures such as color correction, segmentation and tongue's substance-coating separation. This paper presents a novel method to recognize substance and coating from tongue images and eliminate the tongue coating for accurate substance color measurement for diagnosis. By utilizing Hue, Saturation, Value (HSV) color space, new color-brightness threshold parameters have been devised to improve the efficiency of tongue's substance and coating separation procedures and eliminate shadows. The algorithm offers fast processing time around 0.98 seconds for 60,000 pixels tongue image. The successful tongue's substance and coating separation rate reported is 90% compared to the labelled data verified by the practitioners. Using 300 tongue images, the substance Lab color measurement with small standard deviation had revealed the effectiveness of this proposed method in computerized tongue diagnosis system.

  19. DAPNe with micro-capillary separatory chemistry-coupled to MALDI-MS for the analysis of polar and non-polar lipid metabolism in one cell

    NASA Astrophysics Data System (ADS)

    Hamilton, Jason S.; Aguilar, Roberto; Petros, Robby A.; Verbeck, Guido F.

    2017-05-01

    The cellular metabolome is considered to be a representation of cellular phenotype and cellular response to changes to internal or external events. Methods to expand the coverage of the expansive physiochemical properties that makeup the metabolome currently utilize multi-step extractions and chromatographic separations prior to chemical detection, leading to lengthy analysis times. In this study, a single-step procedure for the extraction and separation of a sample using a micro-capillary as a separatory funnel to achieve analyte partitioning within an organic/aqueous immiscible solvent system is described. The separated analytes are then spotted for MALDI-MS imaging and distribution ratios are calculated. Initially, the method is applied to standard mixtures for proof of partitioning. The extraction of an individual cell is non-reproducible; therefore, a broad chemical analysis of metabolites is necessary and will be illustrated with the one-cell analysis of a single Snu-5 gastric cancer cell taken from a cellular suspension. The method presented here shows a broad partitioning dynamic range as a single-step method for lipid analysis demonstrating a decrease in ion suppression often present in MALDI analysis of lipids.

  20. Tuberous sclerosis complex surveillance and management: recommendations of the 2012 International Tuberous Sclerosis Complex Consensus Conference.

    PubMed

    Krueger, Darcy A; Northrup, Hope

    2013-10-01

    Tuberous sclerosis complex is a genetic disorder affecting every organ system, but disease manifestations vary significantly among affected individuals. The diverse and varied presentations and progression can be life-threatening with significant impact on cost and quality of life. Current surveillance and management practices are highly variable among region and country, reflective of the fact that last consensus recommendations occurred in 1998 and an updated, comprehensive standard is lacking that incorporates the latest scientific evidence and current best clinical practices. The 2012 International Tuberous Sclerosis Complex Consensus Group, comprising 79 specialists from 14 countries, was organized into 12 separate subcommittees, each led by a clinician with advanced expertise in tuberous sclerosis complex and the relevant medical subspecialty. Each subcommittee focused on a specific disease area with important clinical management implications and was charged with formulating key clinical questions to address within its focus area, reviewing relevant literature, evaluating the strength of data, and providing a recommendation accordingly. The updated consensus recommendations for clinical surveillance and management in tuberous sclerosis complex are summarized here. The recommendations are relevant to the entire lifespan of the patient, from infancy to adulthood, including both individuals where the diagnosis is newly made as well as individuals where the diagnosis already is established. The 2012 International Tuberous Sclerosis Complex Consensus Recommendations provide an evidence-based, standardized approach for optimal clinical care provided for individuals with tuberous sclerosis complex. Copyright © 2013 The Authors. Published by Elsevier Inc. All rights reserved.

  1. Replacement of the International Standard for Tetanus Antitoxin and the Use of the Standard in the Flocculation Test

    PubMed Central

    Spaun, J.; Lyng, J.

    1970-01-01

    Since 1935 the International Unit for Tetanus Antitoxin has been defined as the activity contained in a certain weight of the first International Standard for Tetanus Antitoxin. As stocks of this standard had become depleted, 11 laboratories in 8 countries were requested to participate in a collaborative assay of a preparation proposed as a replacement. The assay results were analysed and presented to the WHO Expert Committee on Biological Standardization in 1969 which established the preparation studied as the second International Standard for Tetanus Antitoxin and defined the International Unit for Tetanus Antitoxin as the activity contained in 0.03384 mg of the second International Standard for Tetanus Antitoxin. This definition would ensure the continuity of the size of this international unit. The analysis of the collaborative studies also showed that the second International Standard for Tetanus Antitoxin has suitable properties for use in the flocculation test for the determination of the antigen content of tetanus toxoids in Lf values. The designation Lf-equivalent is described and the problems relating to the use of this term for the expression of results of in vitro assays are analysed in relation to the use of international units for expressing results of in vivo assays. As the second International Standard for Tetanus Antitoxin has an in vivo/in vitro ratio of 1.4, the Lf-equivalent of this antitoxin is 1.4 times less than its unitage. PMID:5310949

  2. PROCAL: A Set of 40 Peptide Standards for Retention Time Indexing, Column Performance Monitoring, and Collision Energy Calibration.

    PubMed

    Zolg, Daniel Paul; Wilhelm, Mathias; Yu, Peng; Knaute, Tobias; Zerweck, Johannes; Wenschuh, Holger; Reimer, Ulf; Schnatbaum, Karsten; Kuster, Bernhard

    2017-11-01

    Beyond specific applications, such as the relative or absolute quantification of peptides in targeted proteomic experiments, synthetic spike-in peptides are not yet systematically used as internal standards in bottom-up proteomics. A number of retention time standards have been reported that enable chromatographic aligning of multiple LC-MS/MS experiments. However, only few peptides are typically included in such sets limiting the analytical parameters that can be monitored. Here, we describe PROCAL (ProteomeTools Calibration Standard), a set of 40 synthetic peptides that span the entire hydrophobicity range of tryptic digests, enabling not only accurate determination of retention time indices but also monitoring of chromatographic separation performance over time. The fragmentation characteristics of the peptides can also be used to calibrate and compare collision energies between mass spectrometers. The sequences of all selected peptides do not occur in any natural protein, thus eliminating the need for stable isotope labeling. We anticipate that this set of peptides will be useful for multiple purposes in individual laboratories but also aiding the transfer of data acquisition and analysis methods between laboratories, notably the use of spectral libraries. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Separation and detection of VX and its methylphosphonic acid degradation products on a microchip using indirect laser-induced fluorescence.

    PubMed

    Heleg-Shabtai, Vered; Gratziany, Natzach; Liron, Zvi

    2006-05-01

    The application of indirect LIF (IDLIF) technique for on-chip electrophoretic separation and detection of the nerve agent O-ethyl S-[2-(diisopropylamino)ethyl] methylphosphonothiolate (VX) and its major phosphonic degradation products, ethyl methylphosphonic acid (EMPA) and methylphosphonic acid (MPA) was demonstrated. Separation and detection of MPA degradation products of VX and the nerve agent isopropyl methylphosphonofluoridate (GB) are presented. The negatively charged dye eosin was found to be a good fluorescent marker for both the negatively charged phosphonic acids and the positively charged VX, and was chosen as the IDLIF visualization fluorescent dye. Separation and detection of VX, EMPA, and MPA in a simple-cross microchip were completed within less than a minute, and consumed only a 50 pL sample volume. A characteristic system peak that appeared in all IDLIF electropherograms served as an internal standard that increased the reliability of peak identification. The negative peak of both VX and the MPAs is in agreement with indirect detection theory and with previous reports in the literature. The LOD of VX and EMPA by IDLIF was 30 and 37 microM, respectively. Despite the fact that the detection sensitivity is relatively low, the rapid simultaneous on-chip analysis of both VX and its degradation products as well as the separation and detection of the MPA degradation products of both VX and GB, increases detection reliability and may present a choice when sensitivity is not critical compared with speed and simplicity of the assay.

  4. 25 CFR 542.14 - What are the minimum internal control standards for the cage?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for the cage? 542.14 Section 542.14 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.14 What are the minimum internal control standards for the cage? (a) Computer applications. For...

  5. 25 CFR 543.8 - What are the minimum internal control standards for bingo?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for bingo? 543.8 Section 543.8 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.8 What are the minimum internal control standards for bingo? (a) Supervision....

  6. 25 CFR 542.17 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 25 Indians 2 2011-04-01 2011-04-01 false What are the minimum internal control standards for complimentary services or items? 542.17 Section 542.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.17 What are the minimum internal control standards for complimentary...

  7. 25 CFR 542.17 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 2 2012-04-01 2012-04-01 false What are the minimum internal control standards for complimentary services or items? 542.17 Section 542.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.17 What are the minimum internal control standards for complimentary...

  8. 25 CFR 542.17 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for complimentary services or items? 542.17 Section 542.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.17 What are the minimum internal control standards for complimentary...

  9. 25 CFR 543.8 - What are the minimum internal control standards for bingo?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for bingo? 543.8 Section 543.8 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.8 What are the minimum internal control standards for bingo? (a) Supervision....

  10. 25 CFR 542.17 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for complimentary services or items? 542.17 Section 542.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.17 What are the minimum internal control standards for complimentary...

  11. 25 CFR 542.8 - What are the minimum internal control standards for pull tabs?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for pull tabs? 542.8 Section 542.8 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.8 What are the minimum internal control standards for pull tabs? (a) Computer applications. For...

  12. 25 CFR 542.8 - What are the minimum internal control standards for pull tabs?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for pull tabs? 542.8 Section 542.8 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.8 What are the minimum internal control standards for pull tabs? (a) Computer applications. For...

  13. 25 CFR 542.8 - What are the minimum internal control standards for pull tabs?

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 2 2012-04-01 2012-04-01 false What are the minimum internal control standards for pull tabs? 542.8 Section 542.8 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.8 What are the minimum internal control standards for pull tabs? (a) Computer applications. For...

  14. High-Throughput Genetic Analysis and Combinatorial Chiral Separations Based on Capillary Electrophoresis

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

    Zhong, Wenwan

    2003-01-01

    Capillary electrophoresis (CE) offers many advantages over conventional analytical methods, such as speed, simplicity, high resolution, low cost, and small sample consumption, especially for the separation of enantiomers. However, chiral method developments still can be time consuming and tedious. They designed a comprehensive enantioseparation protocol employing neutral and sulfated cyclodextrins as chiral selectors for common basic, neutral, and acidic compounds with a 96-capillary array system. By using only four judiciously chosen separation buffers, successful enantioseparations were achieved for 49 out of 54 test compounds spanning a large variety of pKs and structures. Therefore, unknown compounds can be screened in thismore » manner to identify optimal enantioselective conditions in just one rn. In addition to superior separation efficiency for small molecules, CE is also the most powerful technique for DNA separations. Using the same multiplexed capillary system with UV absorption detection, the sequence of a short DNA template can be acquired without any dye-labels. Two internal standards were utilized to adjust the migration time variations among capillaries, so that the four electropherograms for the A, T, C, G Sanger reactions can be aligned and base calling can be completed with a high level of confidence. the CE separation of DNA can be applied to study differential gene expression as well. Combined with pattern recognition techniques, small variations among electropherograms obtained by the separation of cDNA fragments produced from the total RNA samples of different human tissues can be revealed. These variations reflect the differences in total RNA expression among tissues. Thus, this Ce-based approach can serve as an alternative to the DNA array techniques in gene expression analysis.« less

  15. Correction for isotopic interferences between analyte and internal standard in quantitative mass spectrometry by a nonlinear calibration function.

    PubMed

    Rule, Geoffrey S; Clark, Zlatuse D; Yue, Bingfang; Rockwood, Alan L

    2013-04-16

    Stable isotope-labeled internal standards are of great utility in providing accurate quantitation in mass spectrometry (MS). An implicit assumption has been that there is no "cross talk" between signals of the internal standard and the target analyte. In some cases, however, naturally occurring isotopes of the analyte do contribute to the signal of the internal standard. This phenomenon becomes more pronounced for isotopically rich compounds, such as those containing sulfur, chlorine, or bromine, higher molecular weight compounds, and those at high analyte/internal standard concentration ratio. This can create nonlinear calibration behavior that may bias quantitative results. Here, we propose the use of a nonlinear but more accurate fitting of data for these situations that incorporates one or two constants determined experimentally for each analyte/internal standard combination and an adjustable calibration parameter. This fitting provides more accurate quantitation in MS-based assays where contributions from analyte to stable labeled internal standard signal exist. It can also correct for the reverse situation where an analyte is present in the internal standard as an impurity. The practical utility of this approach is described, and by using experimental data, the approach is compared to alternative fits.

  16. 78 FR 28725 - Airworthiness Directives; Spectrolab Nightsun XP Searchlight

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-05-16

    ... helicopter and remaining attached solely by the internal cable harness, or separating totally. This condition... Searchlight/ Gimbal could disconnect from the helicopter and remain attached solely by the internal cable harness or separate totally, resulting in damage to the helicopter or injury to persons on the ground...

  17. 77 FR 58707 - Minimum Internal Control Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-09-21

    ... Gaming Commission 25 CFR Part 543 Minimum Internal Control Standards; Final Rule #0;#0;Federal Register... Control Standards AGENCY: National Indian Gaming Commission, Interior. ACTION: Final rule. SUMMARY: The National Indian Gaming Commission (NIGC) amends its minimum internal control standards for Class II gaming...

  18. 77 FR 43196 - Minimum Internal Control Standards and Technical Standards

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-07-24

    ... NATIONAL INDIAN GAMING COMMISSION 25 CFR Parts 543 and 547 Minimum Internal Control Standards [email protected] . SUPPLEMENTARY INFORMATION: Part 543 addresses minimum internal control standards (MICS) for Class II gaming operations. The regulations require tribes to establish controls and implement...

  19. An international observational study suggests that artificial intelligence for clinical decision support optimizes anemia management in hemodialysis patients.

    PubMed

    Barbieri, Carlo; Molina, Manuel; Ponce, Pedro; Tothova, Monika; Cattinelli, Isabella; Ion Titapiccolo, Jasmine; Mari, Flavio; Amato, Claudia; Leipold, Frank; Wehmeyer, Wolfgang; Stuard, Stefano; Stopper, Andrea; Canaud, Bernard

    2016-08-01

    Managing anemia in hemodialysis patients can be challenging because of competing therapeutic targets and individual variability. Because therapy recommendations provided by a decision support system can benefit both patients and doctors, we evaluated the impact of an artificial intelligence decision support system, the Anemia Control Model (ACM), on anemia outcomes. Based on patient profiles, the ACM was built to recommend suitable erythropoietic-stimulating agent doses. Our retrospective study consisted of a 12-month control phase (standard anemia care), followed by a 12-month observation phase (ACM-guided care) encompassing 752 patients undergoing hemodialysis therapy in 3 NephroCare clinics located in separate countries. The percentage of hemoglobin values on target, the median darbepoetin dose, and individual hemoglobin fluctuation (estimated from the intrapatient hemoglobin standard deviation) were deemed primary outcomes. In the observation phase, median darbepoetin consumption significantly decreased from 0.63 to 0.46 μg/kg/month, whereas on-target hemoglobin values significantly increased from 70.6% to 76.6%, reaching 83.2% when the ACM suggestions were implemented. Moreover, ACM introduction led to a significant decrease in hemoglobin fluctuation (intrapatient standard deviation decreased from 0.95 g/dl to 0.83 g/dl). Thus, ACM support helped improve anemia outcomes of hemodialysis patients, minimizing erythropoietic-stimulating agent use with the potential to reduce the cost of treatment. Copyright © 2016 International Society of Nephrology. Published by Elsevier Inc. All rights reserved.

  20. Ensuring Quality in AFRINEST and SATT

    PubMed Central

    2013-01-01

    Background: Three randomized open-label clinical trials [Simplified Antibiotic Therapy Trial (SATT) Bangladesh, SATT Pakistan and African Neonatal Sepsis Trial (AFRINEST)] were developed to test the equivalence of simplified antibiotic regimens compared with the standard regimen of 7 days of parenteral antibiotics. These trials were originally conceived and designed separately; subsequently, significant efforts were made to develop and implement a common protocol and approach. Previous articles in this supplement briefly describe the specific quality control methods used in the individual trials; this article presents additional information about the systematic approaches used to minimize threats to validity and ensure quality across the trials. Methods: A critical component of quality control for AFRINEST and SATT was striving to eliminate variation in clinical assessments and decisions regarding eligibility, enrollment and treatment outcomes. Ensuring appropriate and consistent clinical judgment was accomplished through standardized approaches applied across the trials, including training, assessment of clinical skills and refresher training. Standardized monitoring procedures were also applied across the trials, including routine (day-to-day) internal monitoring of performance and adherence to protocols, systematic external monitoring by funding agencies and external monitoring by experienced, independent trial monitors. A group of independent experts (Technical Steering Committee/Technical Advisory Group) provided regular monitoring and technical oversight for the trials. Conclusions: Harmonization of AFRINEST and SATT have helped to ensure consistency and quality of implementation, both internally and across the trials as a whole, thereby minimizing potential threats to the validity of the trials’ results. PMID:23945575

  1. The Second International Standard for Penicillin*

    PubMed Central

    Humphrey, J. H.; Mussett, M. V.; Perry, W. L. M.

    1953-01-01

    In 1950 the Department of Biological Standards, National Institute for Medical Research, London, was authorized by the WHO Expert Committee on Biological Standardization to prepare the Second International Standard for Penicillin. A single batch of specially recrystallized sodium penicillin G was obtained and 11 laboratories in seven different countries were requested to take part in its collaborative assay. 112 assays were carried out, of which 101 were done by cup-plate methods using either Staphylococcus aureus or Bacillus subtilis. The results were subjected to standard methods of analysis, on the basis of which the authors define the Second International Standard for Penicillin as containing 1,670 International Units (IU) per mg, with limits of error (P = 0.05) of 1,666-1,674 IU/mg. The International Unit is therefore redefined as the activity contained in 0.0005988 mg of the Second International Standard for Penicillin. PMID:13082387

  2. Assessment of Air Quality in the International Space Station (ISS) and Space Shuttle Based on Samples Returned Aboard STS-110 (ISS-8A) in April 2002

    NASA Technical Reports Server (NTRS)

    James, John T.

    2002-01-01

    The toxicological assessment of grab sample canisters (GSCs) returned aboard STS-110 is reported. Analytical methods have not changed from earlier reports, and surrogate standard recoveries from the GSCs were 77-121%, with one exception. Pressure tracking indicated no leaks in the canisters. Recoveries from lab and trip controls for formaldehyde analyses ranged from 87 to 96%. The two general criteria used to assess air quality are the total-non-methane-volatile organic hydrocarbons (NMVOCs) and the total T-value (minus the CO2 and formaldehyde contributions). Because of the inertness of Freon 218 (octafluoropropane, OFP), its contribution to the NMVOC is subtracted and tabulated separately. Control of atmospheric alcohols is important to the water recovery system engineers, hence total alcohols are also shown for each sample. Because formaldehyde is quantified from sorbent badges, its concentration is listed separately. These five indices of air quality are summarized.

  3. Systematic reviews: Separating fact from fiction.

    PubMed

    Haddaway, Neal R; Bilotta, Gary S

    2016-01-01

    The volume of scientific literature continues to expand and decision-makers are faced with increasingly unmanageable volumes of evidence to assess. Systematic reviews (SRs) are powerful tools that aim to provide comprehensive, transparent, reproducible and updateable summaries of evidence. SR methods were developed, and have been employed, in healthcare for more than two decades, and they are now widely used across a broad range of topics, including environmental management and social interventions in crime and justice, education, international development, and social welfare. Despite these successes and the increasing acceptance of SR methods as a 'gold standard' in evidence-informed policy and practice, misconceptions still remain regarding their applicability. The aim of this article is to separate fact from fiction, addressing twelve common misconceptions that can influence the decision as to whether a SR is the most appropriate method for evidence synthesis for a given topic. Through examples, we illustrate the flexibility of SR methods and demonstrate their suitability for addressing issues on environmental health and chemical risk assessment. Copyright © 2015 Elsevier Ltd. All rights reserved.

  4. Notes on Lithology, Mineralogy, and Production for Lunar Simulants

    NASA Technical Reports Server (NTRS)

    Rickman, D. L.; Stoeser, D. B.; Benzel, W. M.; Schrader, C. M.; Edmunson, J. E.

    2011-01-01

    The creation of lunar simulants requires a very broad range of specialized knowledge and information. This document covers several topic areas relevant to lithology, mineralogy, and processing of feedstock materials that are necessary components of the NASA lunar simulant effort. The naming schemes used for both terrestrial and lunar igneous rocks are discussed. The conflict between the International Union of Geological Sciences standard and lunar geology is noted. The rock types known as impactites are introduced. The discussion of lithology is followed by a brief synopsis of pyroxene, plagioclase, and olivine, which are the major mineral constituents of the lunar crust. The remainder of the text addresses processing of materials, particularly the need for separation of feedstock minerals. To illustrate this need, the text includes descriptions of two norite feedstocks for lunar simulants: the Stillwater Complex in Montana, United States, and the Bushveld Complex in South Africa. Magnetic mineral separations, completed by Hazen Research, Inc. and Eriez Manufacturing Co. for the simulant task, are discussed.

  5. High-performance liquid chromatographic separation and electrochemical or spectrophotometric determination of R(-)N-n-propylnorapomorphine and R(-)10,11-methylenedioxy-N-n-propylnoraporphine in primate plasma.

    PubMed

    Lampen, P; Neumeyer, J L; Baldessarini, R J

    1988-04-29

    The dopamine receptor agonist R(-)N-n-propylnorapomorphine (NPA) and its proposed pro-drug R(-)10,11-methylenedioxy-N-n-propylnoraporphine (MDO-NPA) were isolated simultaneously from monkey plasma using a solid-phase extraction procedure. R(-)Apomorphine (APO) and R(-)10,11-methylenedioxyaporphine (MDO-APO) were added as internal standards, and separation and quantification were by high-performance liquid chromatography with electrochemical or ultraviolet detection of the free catechol and MDO compounds, respectively. The detection limits for NPA and MDO-NPA in plasma were 0.5 and 10 ng/ml and the coefficient of variation (S.D./mean) within assays and between days of assays for both drugs was 5.6% or less. Quantification of plasma levels of NPA and MDO-NPA was possible at ranges of 2-1000 and 40-5000 ng/ml, respectively, including concentrations found after intravenous administration of these agents.

  6. 78 FR 54606 - National Emission Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-09-05

    ... Combustion Engines; New Source Performance Standards for Stationary Internal Combustion Engines AGENCY... hazardous air pollutants for stationary reciprocating internal combustion engines and the standards of performance for stationary internal combustion engines. Subsequently, the EPA received three petitions for...

  7. What effect does classroom separation have on twins' behavior, progress at school, and reading abilities?

    PubMed

    Tully, Lucy A; Moffitt, Terrie E; Caspi, Avshalom; Taylor, Alan; Kiernan, Helena; Andreou, Penny

    2004-04-01

    We investigated the effects of classroom separation on twins' behavior, progress at school, and reading abilities. This investigation was part of a longitudinal study of a nationally-representative sample of twins (the E-risk Study) who were assessed at the start of school (age 5) and followed up (age 7). We examined three groups of twins: pairs who were in the same class at both ages; pairs who were in separate classes at both ages; and pairs who were in the same class at age 5, but separated by age 7. When compared to those not separated, those separated early had significantly more teacher-rated internalizing problems and those separated later showed more internalizing problems and lower reading scores. Monozygotic (MZ) twins showed more problems as a result of separation than dizygotic (DZ) twins. No group differences emerged for externalizing problems, ADHD or prosocial behaviors. The implications of the findings for parents and teachers of twins, and for school practices about separating twins, are discussed.

  8. The International Standard for Anti-Brucella abortus Serum

    PubMed Central

    Stableforth, A. W.

    1954-01-01

    In field trials on the eradication of brucellosis from dairy herds in Great Britain, which began in 1933, a serum standard of reference was used for the examination of agglutinating suspensions prepared in different laboratories. In 1937, the Office International des Epizooties (OIE) adopted this standard and made recommendations for its use internationally. These recommendations were revised by OIE in 1948, by the Third Inter-American Congress on Brucellosis and by the Joint FAO/WHO Expert Panel on Brucellosis in 1950, and again by the latter body in 1952. A new batch equivalent in potency to the original standard was established by the WHO Expert Committee on Biological Standardization in 1952 as the International Standard for Anti-Brucella abortus Serum. The International Standard, or a national standard of equivalent potency, ensures comparability of the titres obtained in different countries by different methods, and the results of such comparisons can be expressed in a simple manner by describing the titres in terms of International Units of Brucella antibody. PMID:13199656

  9. Magnetic luminescent nanoparticles as internal calibration for an immunoassay for ricin

    NASA Astrophysics Data System (ADS)

    Dosev, Dosi; Nichkova, Mikaela; Ma, Zhi-Ya; Gee, Shirley J.; Hammock, Bruce D.; Kennedy, Ian M.

    2008-02-01

    Fluorescence techniques rely on measurement of relative fluorescence units and require calibration to obtain reliable and comparable quantitative data. Fluorescent immunoassays are a very sensitive and convenient method of choice for rapid detection of biotoxins, such as ricin. Here we present the application of magnetic luminescent nanoparticles (MLNPs) with a magnetic core of Fe 3O 4 and a fluorescent shell of Eu:Gd IIO 3 as carriers for a nanobead-immunoassay for the detection of ricin with internal calibration. A sandwich immunoassay for ricin was performed on the surface of the MLNPs. The particles were functionalized with capture polyclonal antibodies. Anti-ricin antibodies labeled with Alexa Fluor dye were used as the detecting antibodies. After magnetic extraction, the amount of ricin bound to the particle surface was quantified and related to the fluorescence signal of the nanoparticles. In this new platform, the MLNPs have three main functions: (1) a probe for the specific extraction of the target analyte from the sample; (2) a carrier in the quantitative immunoassay with magnetic separation; and (3) an internal standard in the fluorescence measurement of the dye reporter. The MLNPs serve as an internal control for the total analysis including extraction and assay performance. This approach eliminates the experimental error inherent in particle extraction and measurement of absolute organic dye fluorescence intensities. All fluorescent measurements were performed in a microplate reader. The standard curve for ricin had a dynamic range from 20 ng/ml to 100 μg/ml with a detection limit of 5 ng/ml. The configuration that has been developed can be easily adapted to a high throughput miniaturized system.

  10. [The use of "cognitive" in health terminology. A latent controversy].

    PubMed

    Salvador-Carulla, Luis; Aguilera, Francisco

    2010-10-01

    The adjective «cognitive» has a double meaning and it is used for naming two disciplines with separate activities: Cognitive neuroscience and cognitive psychotherapy. This has an unrecognised impact on the health terminology and the classification systems. The current use of this term is reviewed in a series of key dictionaries, scientific books, databases (OldMedline and PsycINFO) and specific web searchers (Google Scholar). The history of this term and its etymology is also reviewed and compared to other alternatives (i.e. noetic) as well as its use in international classifications (e.g. the International Classification of Functioning - ICF). The modern use of the term «cognitive» in Neurosciences can be traced back to Hebb in a 1955 one year before that recorded at official version. The different meaning of this term in psychology can be traced back to the same decade. Departing from the ICF framework of mental functions, «cognitive» can be regarded as a generic term that encompasses both neurocognitive and meta-cognitive functions and should not be used for classification purposes. A hierarchy is suggested for the use of «neurocognitive» in the classification of mental functions. The polysemic use of this name reveals a latent controversy in health sciences which has implications for its use in the international classification systems. There is an need to improve the standard definition and the semantic hierarchy of the term «cognitive», «neurocognitive» and other related terms within the context of International Health Terminology Standards Development Organisation (IHTSO). Copyright © 2010 SEP y SEPB. Published by Elsevier Espana. All rights reserved.

  11. Rapid determination of methadone and its major metabolite in biological fluids by gas-liquid chromatography with thermionic detection for maintenance treatment of opiate addicts.

    PubMed

    Chikhi-Chorfi, N; Pham-Huy, C; Galons, H; Manuel, N; Lowenstein, W; Warnet, J M; Claude, J R

    1998-11-06

    A rapid gas-liquid chromatographic assay is developed for the quantification of methadone (Mtd) and its major metabolite, 2-ethylidene-1,5-dimethyl-3,3-diphenylpyrrolidine (EDDP), in biological fluids of opiate addicts. After alkaline extraction from samples with lidocaine hydrochloride as internal standard, Mtd and EDDP are separated on SP-2250 column at 220 degrees C and detected with a thermionic detector. The chromatographic time is about 6 min. The relative standard deviations (R.S.D.) of Mtd and EDDP standards are between 1.5 and 5.5%. Most drugs of abuse (morphine, codeine, narcotine, cocaine, benzoylecgonine, cocaethylene, dextropropoxyphene etc) are shown not to interfere with this technique. The method has been applied to study the levels of Mtd and EDDP metabolite in serum, saliva and urine of patients under maintenance treatment for opiate dependence. EDDP levels were found higher than those of Mtd in urine samples from four treated patients, but lower in serum and undetectable in saliva. However, Mtd concentrations were higher in saliva than in serum.

  12. Electronic Procedures for Medical Operations

    NASA Technical Reports Server (NTRS)

    2015-01-01

    Electronic procedures are replacing text-based documents for recording the steps in performing medical operations aboard the International Space Station. S&K Aerospace, LLC, has developed a content-based electronic system-based on the Extensible Markup Language (XML) standard-that separates text from formatting standards and tags items contained in procedures so they can be recognized by other electronic systems. For example, to change a standard format, electronic procedures are changed in a single batch process, and the entire body of procedures will have the new format. Procedures can be quickly searched to determine which are affected by software and hardware changes. Similarly, procedures are easily shared with other electronic systems. The system also enables real-time data capture and automatic bookmarking of current procedure steps. In Phase II of the project, S&K Aerospace developed a Procedure Representation Language (PRL) and tools to support the creation and maintenance of electronic procedures for medical operations. The goal is to develop these tools in such a way that new advances can be inserted easily, leading to an eventual medical decision support system.

  13. 25 CFR 543.17 - What are the minimum internal control standards for drop and count?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for drop and count? 543.17 Section 543.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.17 What are the minimum internal control standards for drop and count?...

  14. 25 CFR 543.15 - What are the minimum internal control standards for lines of credit?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for lines of credit? 543.15 Section 543.15 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.15 What are the minimum internal control standards for lines of credi...

  15. 25 CFR 543.9 - What are the minimum internal control standards for pull tabs?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for pull tabs? 543.9 Section 543.9 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.9 What are the minimum internal control standards for pull tabs? (a)...

  16. 25 CFR 543.13 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for complimentary services or items? 543.13 Section 543.13 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.13 What are the minimum internal control standards fo...

  17. 25 CFR 543.9 - What are the minimum internal control standards for pull tabs?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for pull tabs? 543.9 Section 543.9 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.9 What are the minimum internal control standards for pull tabs? (a)...

  18. 25 CFR 543.15 - What are the minimum internal control standards for lines of credit?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for lines of credit? 543.15 Section 543.15 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.15 What are the minimum internal control standards for lines of credi...

  19. 25 CFR 543.17 - What are the minimum internal control standards for drop and count?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for drop and count? 543.17 Section 543.17 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.17 What are the minimum internal control standards for drop and count?...

  20. 25 CFR 543.13 - What are the minimum internal control standards for complimentary services or items?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for complimentary services or items? 543.13 Section 543.13 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.13 What are the minimum internal control standards fo...

  1. Rapid sensitive validated UPLC-MS method for determination of venlafaxine and its metabolite in rat plasma: Application to pharmacokinetic study.

    PubMed

    Dubey, Sunil Kumar; Saha, R N; Jangala, Hemanth; Pasha, S

    2013-12-01

    A new ultra-performance liquid chromatography-electrospray ionization mass spectrometry (UPLC-MS/ESI) method for simultaneous determination of venlafaxine (VEN) and its metabolite O-desmethylvenlafaxine (ODV) in rat plasma has been developed and validated using Venlafaxine d6 as the internal standard. The compounds and internal standard were extracted from plasma by solid phase extraction. The UPLC separation of the analytes was performed on ACQUITY UPLC ® BEH Shield RP18 (1.7 µm, 100 mm×2.1 mm) column, using isocratic elution with mobile phase constituted of water (containing 2 mM ammonium acetate): acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. All of the analytes were eluted within 1.5 min. The compounds were ionized in the electrospray ionization (ESI) ion source of the mass spectrometer, operating in multiple reaction monitoring (MRM) and positive ion mode. The precursor to product ion transitions monitored for VEN, ODV and Venlafaxine d6 were m / z 278.3→121.08, 264.2→107.1 and 284.4→121.0, respectively. The developed and validated method was used for the pharmacokinetic study of VEN in rats.

  2. HPLC-ESI-MS/MS validated method for simultaneous quantification of zopiclone and its metabolites, N-desmethyl zopiclone and zopiclone-N-oxide in human plasma.

    PubMed

    Mistri, Hiren N; Jangid, Arvind G; Pudage, Ashutosh; Shrivastav, Pranav

    2008-03-15

    A simple, selective and sensitive isocratic HPLC method with triple quadrupole mass spectrometry detection has been developed and validated for simultaneous quantification of zopiclone and its metabolites in human plasma. The analytes were extracted using solid phase extraction, separated on Symmetry shield RP8 column (150 mm x 4.6 mm i.d., 3.5 microm particle size) and detected by tandem mass spectrometry with a turbo ion spray interface. Metaxalone was used as an internal standard. The method had a chromatographic run time of 4.5 min and linear calibration curves over the concentration range of 0.5-150 ng/mL for both zopiclone and N-desmethyl zopiclone and 1-150 ng/mL for zopiclone-N-oxide. The intra-batch and inter-batch accuracy and precision evaluated at lower limit of quantification and quality control levels were within 89.5-109.1% and 3.0-14.7%, respectively, for all the analytes. The recoveries calculated for the analytes and internal standard were > or = 90% from spiked plasma samples. The validated method was successfully employed for a comparative bioavailability study after oral administration of 7.5 mg zopiclone (test and reference) to 16 healthy volunteers under fasted condition.

  3. Bioanalytical Method for Carbocisteine in Human Plasma by Using LC-MS/MS: A Pharmacokinetic Application.

    PubMed

    Dhanure, Shivanand; Savalia, Atulkumar; More, Pravinkumar; Shirode, Prashant; Kapse, Kailas; Shah, Virag

    2014-01-01

    A simple, sensitive, and selective LC-MS/MS method was developed and validated for the quantification of carbocisteine in human plasma. Rosiglitazone was used as the internal standard and heparin was used as the anticoagulant. The chromatographic separation was performed by using the Waters Symmetry Shield RP 8, 150 × 3.9 mm, 5 μ column at 40°C with a mobile phase consisting of a mixture of methanol and 0.5% formic acid solution in a 40:60 proportion. The flow rate was 500 μl/min along with a 5 μl injection volume. Protein precipitation was used as the extraction method. Mass spectrometric data were detected in positive ion mode. The MRM mode of the ions for carbocisteine was 180.0 > 89.0 and for rosiglitazone it was 238.1 > 135.1. The method was validated in the concentration curve range of 50.000 ng/mL to 6000.000 ng/mL. The retention times of carbocisteine and the internal standard rosiglitazone were approximately 2.20 and 3.01 min, respectively. The overall run time was 4.50 min. This method was found suitable to analyze human plasma samples for the application in pharmacokinetic and BA/BE studies.

  4. Ion exchange separation of chromium from natural water matrix for stable isotope mass spectrometric analysis

    USGS Publications Warehouse

    Ball, J.W.; Bassett, R.L.

    2000-01-01

    A method has been developed for separating the Cr dissolved in natural water from matrix elements and determination of its stable isotope ratios using solid-source thermal-ionization mass spectrometry (TIMS). The separation method takes advantage of the existence of the oxidized form of Cr as an oxyanion to separate it from interfering cations using anion-exchange chromatography, and of the reduced form of Cr as a positively charged ion to separate it from interfering anions such as sulfate. Subsequent processing of the separated sample eliminates residual organic material for application to a solid source filament. Ratios for 53Cr/52Cr for National Institute of Standards and Technology Standard Reference Material 979 can be measured using the silica gel-boric acid technique with a filament-to-filament standard deviation in the mean 53Cr/52Cr ratio for 50 replicates of 0.00005 or less. (C) 2000 Elsevier Science B.V. All rights reserved.

  5. The applications of a commercial gas/liquid separator coupled with an inductively coupled plasma mass spectrometer

    PubMed Central

    Hitchen, Peter; Hutton, Robert; Tye, Christopher

    1992-01-01

    A commercially available hydride generator, with a novel membrane gas-liquid separator, has been coupled to a new ICPMS instrument which itself features many unique design considerations. Little or no optimization of the mass spectrometer or ionization source was required to obtain excellent analytical data; and a variety of matrices have been analysed. The elements As and Se are usually used to demonstrate the effectiveness of a hydride generation system, and these are of particular importance, bearing in mind potential Ar molecular overlaps with isotopes of interest. The flexibility of the hydride generation ICP-MS system is highlighted, with the inclusion of analytical figures of merit for the elements Sn, Sb, Ge and Hg, as well as As and Se. Data obtained by ‘standard’ pneumatic nebulization on the ICP-MS is compared with that obtained with the hydride generator for all of the elements. Improvements of between 50 and 100 times were gained in measurements of three sigma detection limits for all elements in the determinations, including Hg. Measurements were made on several isotopes for particular elements, and the data is included for the purposes of comparison. Stabilities of between 1 and 2.5% were obtained for 0.5 ppb solutions over 10 min measurement periods, all data is presented without using an internal standard. Finally, analytical data from seawater standards, spiked with low levels of As and Se and calibrated against aqueous standards, demonstrate excellent recoveries. This is of particular interest bearing in mind the well-documented molecular interferences from high chloride matrices on As and Se analysis. PMID:18924920

  6. 26 CFR 1.663(c)-3 - Applicability of separate share rule to certain trusts.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... under applicable law do not constitute separate trusts) for each of the testator's children and the... trusts. 1.663(c)-3 Section 1.663(c)-3 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES Estates and Trusts Which May Accumulate Income Or...

  7. Laparoscopic versus open-component separation: a comparative analysis in a porcine model.

    PubMed

    Rosen, Michael J; Williams, Christina; Jin, Judy; McGee, Michael F; Schomisch, Steve; Marks, Jeffrey; Ponsky, Jeffrey

    2007-09-01

    The ideal surgical treatment for complicated ventral hernias remains elusive. Traditional component separation provides local advancement of native tissue for tension-free closure without prosthetic materials. This technique requires an extensive subcutaneous dissection with division of perforating vessels predisposing to skin-flap necrosis and complicated wound infections. A minimally invasive component separation may decrease wound complication rates; however, the adequacy of the myofascial advancement has not been studied. Five 25-kg pigs underwent bilateral laparoscopic component separation. A 10-mm incision was made lateral to the rectus abdominus muscle. The external oblique fascia was incised, and a dissecting balloon was inflated between the internal and external oblique muscles. Two additional ports were placed in the intermuscular space. The external oblique was incised from the costal margin to the inguinal ligament. The maximal abdominal wall advancement was recorded. A formal open-component separation was performed and maximal advancement 5 cm superior and 5 cm inferior to the umbilicus was recorded for comparison. Groups were compared using standard statistical analysis. The laparoscopic component separation was completed successfully in all animals, with a mean of 22 min/side. Laparoscopic component separation yielded 3.9 cm (SD 1.1) of fascial advancement above the umbilicus, whereas 4.4 cm (1.2) was obtained after open release (P = .24). Below the umbilicus, laparoscopic release achieved 5.0 cm (1.0) of advancement, whereas 5.8 cm (1.2) was gained after open release (P = .13). The minimally invasive component separation achieved an average of 86% of the myofascial advancement compared with a formal open release. The laparoscopic approach does not require extensive subcutaneous dissection and might theoretically result in a decreased incidence or decreased complexity of postoperative wound infections or skin-flap necrosis. Based on our preliminary data in this porcine model, further comparative studies of laparoscopic versus open component separation in complex ventral hernia repair is warranted to evaluate postoperative morbidity and long-term hernia recurrence rates.

  8. Method and apparatus for processing a test sample to concentrate an analyte in the sample from a solvent in the sample

    DOEpatents

    Turner, Terry D.; Beller, Laurence S.; Clark, Michael L.; Klingler, Kerry M.

    1997-01-01

    A method of processing a test sample to concentrate an analyte in the sample from a solvent in the sample includes: a) boiling the test sample containing the analyte and solvent in a boiling chamber to a temperature greater than or equal to the solvent boiling temperature and less than the analyte boiling temperature to form a rising sample vapor mixture; b) passing the sample vapor mixture from the boiling chamber to an elongated primary separation tube, the separation tube having internal sidewalls and a longitudinal axis, the longitudinal axis being angled between vertical and horizontal and thus having an upper region and a lower region; c) collecting the physically transported liquid analyte on the internal sidewalls of the separation tube; and d) flowing the collected analyte along the angled internal sidewalls of the separation tube to and pass the separation tube lower region. The invention also includes passing a turbulence inducing wave through a vapor mixture to separate physically transported liquid second material from vaporized first material. Apparatus are also disclosed for effecting separations. Further disclosed is a fluidically powered liquid test sample withdrawal apparatus for withdrawing a liquid test sample from a test sample container and for cleaning the test sample container.

  9. Method and apparatus for processing a test sample to concentrate an analyte in the sample from a solvent in the sample

    DOEpatents

    Turner, T.D.; Beller, L.S.; Clark, M.L.; Klingler, K.M.

    1997-10-14

    A method of processing a test sample to concentrate an analyte in the sample from a solvent in the sample includes: (a) boiling the test sample containing the analyte and solvent in a boiling chamber to a temperature greater than or equal to the solvent boiling temperature and less than the analyte boiling temperature to form a rising sample vapor mixture; (b) passing the sample vapor mixture from the boiling chamber to an elongated primary separation tube, the separation tube having internal sidewalls and a longitudinal axis, the longitudinal axis being angled between vertical and horizontal and thus having an upper region and a lower region; (c) collecting the physically transported liquid analyte on the internal sidewalls of the separation tube; and (d) flowing the collected analyte along the angled internal sidewalls of the separation tube to and pass the separation tube lower region. The invention also includes passing a turbulence inducing wave through a vapor mixture to separate physically transported liquid second material from vaporized first material. Apparatus is also disclosed for effecting separations. Further disclosed is a fluidically powered liquid test sample withdrawal apparatus for withdrawing a liquid test sample from a test sample container and for cleaning the test sample container. 8 figs.

  10. Child temperament moderates the impact of parental separation on adolescent mental health: The trails study.

    PubMed

    Sentse, Miranda; Ormel, Johan; Veenstra, René; Verhulst, Frank C; Oldehinkel, Albertine J

    2011-02-01

    The potential effect of parental separation during early adolescence on adolescent externalizing and internalizing problems was investigated in a longitudinal sample of adolescents (n = 1274; mean age = 16.27; 52.3% girls). Pre-separation mental health problems were controlled for. Building on a large number of studies that overall showed a small effect of parental separation, it was argued that separation may only or especially have an effect under certain conditions. It was examined whether child temperament (effortful control and fearfulness) moderates the impact of parental separation on specific mental health domains. Hypotheses were derived from a goal-framing theory, with a focus on goals related to satisfying the need for autonomy and the need to belong. Controlling for the overlap between the outcome domains, we found that parental separation led to an increase in externalizing problems but not internalizing problems when interactions with child temperament were ignored. Moreover, child temperament moderated the impact of parental separation, in that it was only related to increased externalizing problems for children low on effortful control, whereas it was only related to increased internalizing problems for children high on fearfulness. The results indicate that person-environment interactions are important for understanding the development of mental health problems and that these interactions can be domain-specific. PsycINFO Database Record (c) 2011 APA, all rights reserved.

  11. Prescription, Dispensation, and Generic Medicine Replacement Ratios: Influence on Japanese Medicine Costs

    PubMed Central

    Yokoi, Masayuki; Tashiro, Takao

    2016-01-01

    This study used publicly available data to examine the effect of the separation of dispensing and prescribing medicines between pharmacists in pharmacies and doctors in medical institutions (the separation system) and the generic medicine replacement ratio on the cost of various medicines in Japanese prefectures. For Japanese medical institutions, participation in the separation system is optional. Consequently, the expansion rate of the separation system for each administrative district is highly variable. In our multiple regression analysis, the dependent variables were the costs of daily medicines, specifically, total, internal, external, and injection medicines, as well as medical devices, and the independent variables were the expansion rate of the separation system and generic medicine replacement ratio. The expansion rate of the separation system showed a significant negative partial correlation with the daily costs of total, internal, and injection medicines as well as medical devices. Moreover, the rate of replacing brand name medicines with generic medicines showed a significant negative partial correlation with the daily costs of total and internal medicines. However, external and injection medicines and medical devices did not because only a few or no generic products of these types were sold in the Japanese market. Otherwise, expansion of the separation system was effective in reducing medicine costs, except in the case of external medicines. This suggests that the cost efficiency effect of the separation system does not function all the time. PMID:26234979

  12. 26 CFR 26.2654-1 - Certain trusts treated as separate trusts.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 14 2010-04-01 2010-04-01 false Certain trusts treated as separate trusts. 26... 1986 § 26.2654-1 Certain trusts treated as separate trusts. (a) Single trust treated as separate trusts—(1) Substantially separate and independent shares—(i) In general. If a single trust consists solely...

  13. Steroid isotopic standards for gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS).

    PubMed

    Zhang, Ying; Tobias, Herbert J; Brenna, J Thomas

    2009-03-01

    Carbon isotope ratio (CIR) analysis of urinary steroids using gas chromatography-combustion isotope ratio mass spectrometry (GCC-IRMS) is a recognized test to detect illicit doping with synthetic testosterone. There are currently no universally used steroid isotopic standards (SIS). We adapted a protocol to prepare isotopically uniform steroids for use as a calibrant in GCC-IRMS that can be analyzed under the same conditions as used for steroids extracted from urine. Two separate SIS containing a mixture of steroids were created and coded CU/USADA 33-1 and CU/USADA 34-1, containing acetates and native steroids, respectively. CU/USADA 33-1 contains 5alpha-androstan-3beta-ol acetate (5alpha-A-AC), 5alpha-androstan-3alpha-ol-17-one acetate (androsterone acetate, A-AC), 5beta-androstan-3alpha-ol-11, 17-dione acetate (11-ketoetiocholanolone acetate, 11k-AC) and 5alpha-cholestane (Cne). CU/USADA 34-1 contains 5beta-androstan-3alpha-ol-17-one (etiocholanolone, E), 5alpha-androstan-3alpha-ol-17-one (androsterone, A), and 5beta-pregnane-3alpha, 20alpha-diol (5betaP). Each mixture was prepared and dispensed into a set of about 100 ampoules using a protocol carefully designed to minimize isotopic fractionation and contamination. A natural gas reference material, NIST RM 8559, traceable to the international standard Vienna PeeDee Belemnite (VPDB) was used to calibrate the SIS. Absolute delta(13)C(VPDB) and Deltadelta(13)C(VPDB) values from randomly selected ampoules from both SIS indicate uniformity of steroid isotopic composition within measurement reproducibility, SD(delta(13)C)<0.2 per thousand. This procedure for creation of isotopic steroid mixtures results in consistent standards with isotope ratios traceable to the relevant international reference material.

  14. A quantitative liquid chromatography tandem mass spectrometry method for metabolomic analysis of Plasmodium falciparum lipid related metabolites.

    PubMed

    Vo Duy, S; Besteiro, S; Berry, L; Perigaud, C; Bressolle, F; Vial, H J; Lefebvre-Tournier, I

    2012-08-20

    Plasmodium falciparum is the causative agent of malaria, a deadly infectious disease for which treatments are scarce and drug-resistant parasites are now increasingly found. A comprehensive method of identifying and quantifying metabolites of this intracellular parasite could expand the arsenal of tools to understand its biology, and be used to develop new treatments against the disease. Here, we present two methods based on liquid chromatography tandem mass spectrometry for reliable measurement of water-soluble metabolites involved in phospholipid biosynthesis, as well as several other metabolites that reflect the metabolic status of the parasite including amino acids, carboxylic acids, energy-related carbohydrates, and nucleotides. A total of 35 compounds was quantified. In the first method, polar compounds were retained by hydrophilic interaction chromatography (amino column) and detected in negative mode using succinic acid-(13)C(4) and fluorovaline as internal standards. In the second method, separations were carried out using reverse phase (C18) ion-pair liquid chromatography, with heptafluorobutyric acid as a volatile ion pairing reagent in positive detection mode, using d(9)-choline and 4-aminobutanol as internal standards. Standard curves were performed in P. falciparum-infected and uninfected red blood cells using standard addition method (r(2)>0.99). The intra- and inter-day accuracy and precision as well as the extraction recovery of each compound were determined. The lower limit of quantitation varied from 50pmol to 100fmol/3×10(7)cells. These methods were validated and successfully applied to determine intracellular concentrations of metabolites from uninfected host RBCs and isolated Plasmodium parasites. Copyright © 2012 Elsevier B.V. All rights reserved.

  15. Stability indicating validated HPLC method for quantification of levothyroxine with eight degradation peaks in the presence of excipients.

    PubMed

    Shah, R B; Bryant, A; Collier, J; Habib, M J; Khan, M A

    2008-08-06

    A simple, sensitive, accurate, and robust stability indicating analytical method is presented for identification, separation, and quantitation of l-thyroxine and eight degradation impurities with an internal standard. The method was used in the presence of commonly used formulation excipients such as butylated hydroxyanisole, povidone, crospovidone, croscarmellose sodium, mannitol, sucrose, acacia, lactose monohydrate, confectionary sugar, microcrystalline cellulose, sodium laurel sulfate, magnesium stearate, talc, and silicon dioxide. The two active thyroid hormones: 3,3',5,5'-tetra-iodo-l-thyronine (l-thyroxine-T4) and 3,3',5-tri-iodo-l-thyronine (T3) and degradation products including di-iodothyronine (T2), thyronine (T0), tyrosine (Tyr), di-iodotyrosine (DIT), mono-iodotyrosine (MIT), 3,3',5,5'-tetra-iodothyroacetic acid (T4AA) and 3,3',5-tri-iodothyroacetic acid (T3AA) were assayed by the current method. The separation of l-thyroxine and eight metabolites along with theophylline (internal standard) was achieved using a C18 column (25 degrees C) with a mobile phase of trifluoroacetic acid (0.1%, v/v, pH 3)-acetonitrile in gradient elution at 0.8 ml/min at 223 nm. The sample diluent was 0.01 M methanolic NaOH. Method was validated according to FDA, USP, and ICH guidelines for inter-day accuracy, precision, and robustness after checking performance with system suitability. Tyr (4.97 min), theophylline (9.09 min), MIT (9.55 min), DIT (11.37 min), T0 (11.63 min), T2 (14.47 min), T3 (16.29 min), T4 (17.60 min), T3AA (22.71 min), and T4AA (24.83 min) separated in a single chromatographic run. Linear relationship (r2>0.99) was observed between the peak area ratio and the concentrations for all of the compounds within the range of 2-20 microg/ml. The total time for analysis, equilibration and recovery was 40 min. The method was shown to separate well from commonly employed formulation excipients. Accuracy ranged from 95 to 105% for T4 and 90 to 110% for all other compounds. Precision was <2% for all the compounds. The method was found to be robust with minor changes in injection volume, flow rate, column temperature, and gradient ratio. Validation results indicated that the method shows satisfactory linearity, precision, accuracy, and ruggedness and also stress degradation studies indicated that the method can be used as stability indicating method for l-thyroxine in the presence of excipients.

  16. CTEPP STANDARD OPERATING PROCEDURE FOR PREPARATION OF SURROGATE RECOVERY STANDARD AND INTERNAL STANDARD SOLUTIONS FOR NEUTRAL TARGET ANALYTES (SOP-5.25)

    EPA Science Inventory

    This standard operating procedure describes the method used for preparing internal standard, surrogate recovery standard and calibration standard solutions for neutral analytes used for gas chromatography/mass spectrometry analysis.

  17. An International Urogynecological Association (IUGA)/International Continence Society (ICS) joint report on the terminology for female anorectal dysfunction.

    PubMed

    Sultan, Abdul H; Monga, Ash; Lee, Joseph; Emmanuel, Anton; Norton, Christine; Santoro, Giulio; Hull, Tracy; Berghmans, Bary; Brody, Stuart; Haylen, Bernard T

    2017-01-01

    The terminology for anorectal dysfunction in women has long been in need of a specific clinically-based Consensus Report. This Report combines the input of members of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA) and the International Continence Society (ICS), assisted on Committee by experts in their fields to form a Joint IUGA/ICS Working Group on Female Anorectal Terminology. Appropriate core clinical categories and sub classifications were developed to give an alphanumeric coding to each definition. An extensive process of twenty rounds of internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). A Terminology Report for anorectal dysfunction, encompassing over 130 separate definitions, has been developed. It is clinically based with the most common diagnoses defined. Clarity and user-friendliness have been key aims to make it interpretable by practitioners and trainees in all the different specialty groups involved in female pelvic floor dysfunction. Female-specific anorectal investigations and imaging (ultrasound, radiology and MRI) has been included whilst appropriate figures have been included to supplement and help clarify the text. Interval review (5-10 years) is anticipated to keep the document updated and as widely acceptable as possible. A consensus-based Terminology Report for female anorectal dysfunction terminology has been produced aimed at being a significant aid to clinical practice and a stimulus for research. Neurourol. Urodynam. 36:10-34, 2017. © 2016 Wiley Periodicals, Inc., and The International Urogynecological Association. © 2016 Wiley Periodicals, Inc., and The International Urogynecological Association.

  18. Quantification and statistical significance analysis of group separation in NMR-based metabonomics studies

    PubMed Central

    Goodpaster, Aaron M.; Kennedy, Michael A.

    2015-01-01

    Currently, no standard metrics are used to quantify cluster separation in PCA or PLS-DA scores plots for metabonomics studies or to determine if cluster separation is statistically significant. Lack of such measures makes it virtually impossible to compare independent or inter-laboratory studies and can lead to confusion in the metabonomics literature when authors putatively identify metabolites distinguishing classes of samples based on visual and qualitative inspection of scores plots that exhibit marginal separation. While previous papers have addressed quantification of cluster separation in PCA scores plots, none have advocated routine use of a quantitative measure of separation that is supported by a standard and rigorous assessment of whether or not the cluster separation is statistically significant. Here quantification and statistical significance of separation of group centroids in PCA and PLS-DA scores plots are considered. The Mahalanobis distance is used to quantify the distance between group centroids, and the two-sample Hotelling's T2 test is computed for the data, related to an F-statistic, and then an F-test is applied to determine if the cluster separation is statistically significant. We demonstrate the value of this approach using four datasets containing various degrees of separation, ranging from groups that had no apparent visual cluster separation to groups that had no visual cluster overlap. Widespread adoption of such concrete metrics to quantify and evaluate the statistical significance of PCA and PLS-DA cluster separation would help standardize reporting of metabonomics data. PMID:26246647

  19. Break modeling for RELAP5 analyses of ISP-27 Bethsy

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

    Petelin, S.; Gortnar, O.; Mavko, B.

    This paper presents pre- and posttest analyses of International Standard Problem (ISP) 27 on the Bethsy facility and separate RELAP5 break model tests considering the measured boundary condition at break inlet. This contribution also demonstrates modifications which have assured the significant improvement of model response in posttest simulations. Calculations were performed using the RELAP5/MOD2/36.05 and RELAP5/MOD3.5M5 codes on the MicroVAX, SUN, and CONVEX computers. Bethsy is an integral test facility that simulates a typical 900-MW (electric) Framatome pressurized water reactor. The ISP-27 scenario involves a 2-in. cold-leg break without HPSI and with delayed operator procedures for secondary system depressurization.

  20. The gallium melting-point standard: a determination of the liquid-solid equilibrium temperature of pure gallium on the International Practical Temperature Scale of 1968.

    PubMed

    Thornton, D D

    1977-01-01

    The sharpness and reproducibility of the gallium melting point were studied and the melting temperature of gallium in terms of IPTS-68 was determined. Small melting-point cells designed for use with thermistors are described. Nine gallium cells including three levels of purity were used in 68 separate determinations fo the melting point. The melting point of 99.99999% pure gallium in terms of IPTS-68 is found to be 29.771(4) +/- 0.001(4) degree C; the melting range is less than 0.0005 degree C and is reproducible to +/- 0.0004 degree C.

  1. Internally folded expanded metal electrode for battery construction

    NASA Technical Reports Server (NTRS)

    Pierce, Doug C. (Inventor); Korinek, Paul D. (Inventor); Morgan, Maurice C. (Inventor)

    1993-01-01

    A battery system is disclosed which includes folded grids of expanded metal inserted through non-conductive substrates and pasted with electrochemically active materials. In the most preferred embodiment, a frame is provided with a plastic insert, and slots are provided in the latter to receive the expanded metal grid. After suitable coinage of the grid and insertion through the plastic film, the grid is sealed and pasted on opposite sides with positive and negative active material. A battery is assembled using one or a plurality of the resulting electrode elements, with separators, to produce a high-power, lead-acid battery. The folded grid provides many of the design benefits of standard bipolar construction.

  2. International Standardization of Bed Rest Standard Measures

    NASA Technical Reports Server (NTRS)

    Cromwell, Ronita L.

    2010-01-01

    This slide presentation gives an overview of the standardization of bed rest measures. The International Countermeasures Working Group attempted to define and agree internationally on standard measurements for spaceflight based bed rest studies. The group identified the experts amongst several stakeholder agencys. It included information on exercise, muscle, neurological, psychological, bone and cardiovascular measures.

  3. Metrics for comparing plasma mass filters

    NASA Astrophysics Data System (ADS)

    Fetterman, Abraham J.; Fisch, Nathaniel J.

    2011-10-01

    High-throughput mass separation of nuclear waste may be useful for optimal storage, disposal, or environmental remediation. The most dangerous part of nuclear waste is the fission product, which produces most of the heat and medium-term radiation. Plasmas are well-suited to separating nuclear waste because they can separate many different species in a single step. A number of plasma devices have been designed for such mass separation, but there has been no standardized comparison between these devices. We define a standard metric, the separative power per unit volume, and derive it for three different plasma mass filters: the plasma centrifuge, Ohkawa filter, and the magnetic centrifugal mass filter.

  4. Blind Source Separation of Seismic Events with Independent Component Analysis: CTBT related exercise

    NASA Astrophysics Data System (ADS)

    Rozhkov, Mikhail; Kitov, Ivan

    2015-04-01

    Blind Source Separation (BSS) methods used in signal recovery applications are attractive for they use minimal a priori information about the signals they are dealing with. Homomorphic deconvolution and cepstrum estimation are probably the only methods used in certain extent in CTBT applications that can be attributed to the given branch of technology. However Expert Technical Analysis (ETA) conducted in CTBTO to improve the estimated values for the standard signal and event parameters according to the Protocol to the CTBT may face problems which cannot be resolved with certified CTBTO applications and may demand specific techniques not presently used. The problem to be considered within the ETA framework is the unambiguous separation of signals with close arrival times. Here, we examine two scenarios of interest: (1) separation of two almost co-located explosions conducted within fractions of seconds, and (2) extraction of explosion signals merged with wavetrains from strong earthquake. The importance of resolving the problem related to case 1 is connected with the correct explosion yield estimation. Case 2 is a well-known scenario of conducting clandestine nuclear tests. While the first case can be approached somehow with the means of cepstral methods, the second case can hardly be resolved with the conventional methods implemented at the International Data Centre, especially if the signals have close slowness and azimuth. Independent Component Analysis (in its FastICA implementation) implying non-Gaussianity of the underlying processes signal's mixture is a blind source separation method that we apply to resolve the mentioned above problems. We have tested this technique with synthetic waveforms, seismic data from DPRK explosions and mining blasts conducted within East-European platform as well as with signals from strong teleseismic events (Sumatra, April 2012 Mw=8.6, and Tohoku, March 2011 Mw=9.0 earthquakes). The data was recorded by seismic arrays of the International Monitoring System of CTBTO and by small-aperture seismic array Mikhnevo (MHVAR) operated by the Institute of Geosphere Dynamics, Russian Academy of Sciences. Our approach demonstrated a good ability of separation of seismic sources with very close origin times and locations (hundreds of meters), and/or having close arrival times (fractions of seconds), and recovering their waveforms from the mixture. Perspectives and limitations of the method are discussed.

  5. The International Standard for Aureomycin

    PubMed Central

    Humphrey, J. H.; Lightbown, J. W.; Mussett, M. V.; Perry, W. L. M.

    1953-01-01

    In 1950, the Department of Biological Standards, National Institute for Medical Research, London, was authorized by the WHO Expert Committee on Biological Standardization to proceed with the establishment of an International Standard for Aureomycin. A 100-g batch of aureomycin was obtained and was compared with the Standard Preparation of Aureomycin of the United States Food and Drug Administration (FDA) in a collaborative assay in which six laboratories in five countries participated. In all, 30 assays were carried out; 26 of these were done by biological methods, using Sarcina lutea, Bacillus pumilus, Staphylococcus aureus, or Bacillus cereus, and the remaining four by physicochemical methods. The results were subjected to standard methods of analysis, and the overall weighted mean potency (calculated from the biological assays only) was 1.0139, with limits of error of 99.5% to 100.5%. Since the International Standard is 1.39% more potent than the FDA Standard Preparation, it is probable that the latter contains a small amount of inert material; it is also possible that the International Standard itself is not 100% pure. For most practical purposes, however, both preparations may be regarded as substantially pure, and it is considered that to alter the present practice of quoting aureomycin dosage in metric units of weight would be inadvisable. Nevertheless, since the International Standard may not be a pure substance, a unit notation—for use where required in bioassays—is desirable, and the International Unit of Aureomycin has therefore been defined as the activity contained in one microgram of the International Standard. PMID:13141137

  6. Assessing the properties of internal standards for quantitative matrix-assisted laser desorption/ionization mass spectrometry of small molecules.

    PubMed

    Sleno, Lekha; Volmer, Dietrich A

    2006-01-01

    Growing interest in the ability to conduct quantitative assays for small molecules by matrix-assisted laser desorption/ionization (MALDI) has been the driving force for several recent studies. This present work includes the investigation of internal standards for these analyses using a high-repetition rate MALDI triple quadrupole instrument. Certain physicochemical properties are assessed for predicting possible matches for internal standards for different small molecules. The importance of similar molecular weight of an internal standard to its analyte is seen through experiments with a series of acylcarnitines, having a fixed charge site and growing alkyl chain length. Both acetyl- and hexanoyl-carnitine were systematically assessed with several other acylcarnitine compounds as internal standards. The results clearly demonstrate that closely matched molecular weights between analyte and internal standard are essential for acceptable quantitation results. Using alpha-cyano-4-hydroxycinnamic acid as the organic matrix, the similarities between analyte and internal standard remain the most important parameter and not necessarily their even distribution within the solid sample spot. Several 4-quinolone antibiotics as well as a diverse group of pharmaceutical drugs were tested as internal standards for the 4-quinolone, ciprofloxacin. Quantitative results were shown using the solution-phase properties, log D and pKa, of these molecules. Their distribution coefficients, log D, are demonstrated as a fundamental parameter for similar crystallization patterns of analyte and internal standard. In the end, it was also possible to quantify ciprofloxacin using a drug from a different compound class, namely quinidine, having a similar log D value as the analyte. Copyright 2006 John Wiley & Sons, Ltd.

  7. 26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT..., Stock Bonus Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating...

  8. 26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT..., Stock Bonus Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating...

  9. 26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT... Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating qualified...

  10. 26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT..., Stock Bonus Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating...

  11. 26 CFR 1.414(r)-1 - Requirements applicable to qualified separate lines of business.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... lines of business. 1.414(r)-1 Section 1.414(r)-1 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT..., Stock Bonus Plans, Etc. § 1.414(r)-1 Requirements applicable to qualified separate lines of business. (a) In general. Section 414(r) prescribes the conditions under which an employer is treated as operating...

  12. Parental Separation and Child Aggressive and Internalizing Behavior: An Event History Calendar Analysis

    ERIC Educational Resources Information Center

    Averdijk, Margit; Malti, Tina; Eisner, Manuel; Ribeaud, Denis

    2012-01-01

    This study investigated the relationship between parental separation and aggressive and internalizing behavior in a large sample of Swiss children drawn from the ongoing Zurich Project on the Social Development of Children and Youths. Parents retrospectively reported life events and problem behavior for the first 7 years of the child's life on a…

  13. Analysis of rare earth elements in coal fly ash using laser ablation inductively coupled plasma mass spectrometry and scanning electron microscopy

    NASA Astrophysics Data System (ADS)

    Thompson, Robert L.; Bank, Tracy; Montross, Scott; Roth, Elliot; Howard, Bret; Verba, Circe; Granite, Evan

    2018-05-01

    Reference standard NIST SRM 1633b and FA 345, a fly ash sample from an eastern U.S. coal power plant, were analyzed to determine and quantify the mineralogical association of rare earth elements (REE). These analyses were completed using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and a scanning electron microscope, equipped with an energy-dispersive X-ray spectrometer (SEM-EDS). Internal standardization was avoided by quantifying elemental concentrations by normalizing to 100% oxides. Mineral grains containing elevated REE concentrations were found in diverse chemical environments, but were most commonly found in regions where Al and Si were predominant. Dividing the spot analyses into time segments yielded plots that showed the REE content changing over time as individual mineral grains were being ablated. SEM-EDS images of FA 345 confirmed the trends that were found in the LA-ICP-MS results. Small grains of apatite, monazite, or zircon were frequently observed as free mineral grains or embedded in amorphous aluminosilicate glass and were not associated with ferrous particles. This finding is consistent with previous reports that magnetic enrichment may be an effective way of concentrating non-magnetic REE phases. Furthermore, aggressive mechanical and chemical-based separation schemes will be required to separate and recover REE from aluminosilicate glass.

  14. Standardized Full-Field Electroretinography in the Green Monkey (Chlorocebus sabaeus)

    PubMed Central

    Bouskila, Joseph; Javadi, Pasha; Palmour, Roberta M.; Bouchard, Jean-François; Ptito, Maurice

    2014-01-01

    Abstract Full-field electroretinography is an objective measure of retinal function, serving as an important diagnostic clinical tool in ophthalmology for evaluating the integrity of the retina. Given the similarity between the anatomy and physiology of the human and Green Monkey eyes, this species has increasingly become a favorable non-human primate model for assessing ocular defects in humans. To test this model, we obtained full-field electroretinographic recordings (ERG) and normal values for standard responses required by the International Society for Clinical Electrophysiology of Vision (ISCEV). Photopic and scotopic ERG recordings were obtained by full-field stimulation over a range of 6 log units of intensity in dark-adapted or light-adapted eyes of adult Green Monkeys (Chlorocebus sabaeus). Intensity, duration, and interval of light stimuli were varied separately. Reproducible values of amplitude and latency were obtained for the a- and b-waves, under well-controlled adaptation and stimulus conditions; the i-wave was also easily identifiable and separated from the a-b-wave complex in the photopic ERG. The recordings obtained in the healthy Green Monkey matched very well with those in humans and other non-human primate species (Macaca mulatta and Macaca fascicularis). These results validate the Green Monkey as an excellent non-human primate model, with potential to serve for testing retinal function following various manipulations such as visual deprivation or drug evaluation. PMID:25360686

  15. International collaborative study for the calibration of proposed International Standards for thromboplastin, rabbit, plain, and for thromboplastin, recombinant, human, plain.

    PubMed

    van den Besselaar, A M H P; Chantarangkul, V; Angeloni, F; Binder, N B; Byrne, M; Dauer, R; Gudmundsdottir, B R; Jespersen, J; Kitchen, S; Legnani, C; Lindahl, T L; Manning, R A; Martinuzzo, M; Panes, O; Pengo, V; Riddell, A; Subramanian, S; Szederjesi, A; Tantanate, C; Herbel, P; Tripodi, A

    2018-01-01

    Essentials Two candidate International Standards for thromboplastin (coded RBT/16 and rTF/16) are proposed. International Sensitivity Index (ISI) of proposed standards was assessed in a 20-centre study. The mean ISI for RBT/16 was 1.21 with a between-centre coefficient of variation of 4.6%. The mean ISI for rTF/16 was 1.11 with a between-centre coefficient of variation of 5.7%. Background The availability of International Standards for thromboplastin is essential for the calibration of routine reagents and hence the calculation of the International Normalized Ratio (INR). Stocks of the current Fourth International Standards are running low. Candidate replacement materials have been prepared. This article describes the calibration of the proposed Fifth International Standards for thromboplastin, rabbit, plain (coded RBT/16) and for thromboplastin, recombinant, human, plain (coded rTF/16). Methods An international collaborative study was carried out for the assignment of International Sensitivity Indexes (ISIs) to the candidate materials, according to the World Health Organization (WHO) guidelines for thromboplastins and plasma used to control oral anticoagulant therapy with vitamin K antagonists. Results Results were obtained from 20 laboratories. In several cases, deviations from the ISI calibration model were observed, but the average INR deviation attributabled to the model was not greater than 10%. Only valid ISI assessments were used to calculate the mean ISI for each candidate. The mean ISI for RBT/16 was 1.21 (between-laboratory coefficient of variation [CV]: 4.6%), and the mean ISI for rTF/16 was 1.11 (between-laboratory CV: 5.7%). Conclusions The between-laboratory variation of the ISI for candidate material RBT/16 was similar to that of the Fourth International Standard (RBT/05), and the between-laboratory variation of the ISI for candidate material rTF/16 was slightly higher than that of the Fourth International Standard (rTF/09). The candidate materials have been accepted by WHO as the Fifth International Standards for thromboplastin, rabbit plain, and thromboplastin, recombinant, human, plain. © 2017 International Society on Thrombosis and Haemostasis.

  16. 22 CFR 41.24 - International organization aliens.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 22 Foreign Relations 1 2014-04-01 2014-04-01 false International organization aliens. 41.24... aliens. (a) Definition of international organization. “International organization” means: (1) Any public...)(27)(I), INTELSAT or any successor or separated entity thereof. (b) Aliens coming to international...

  17. 22 CFR 41.24 - International organization aliens.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 22 Foreign Relations 1 2010-04-01 2010-04-01 false International organization aliens. 41.24... aliens. (a) Definition of international organization. “International organization” means: (1) Any public...)(27)(I), INTELSAT or any successor or separated entity thereof. (b) Aliens coming to international...

  18. 22 CFR 41.24 - International organization aliens.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 22 Foreign Relations 1 2012-04-01 2012-04-01 false International organization aliens. 41.24... aliens. (a) Definition of international organization. “International organization” means: (1) Any public...)(27)(I), INTELSAT or any successor or separated entity thereof. (b) Aliens coming to international...

  19. 22 CFR 41.24 - International organization aliens.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 22 Foreign Relations 1 2011-04-01 2011-04-01 false International organization aliens. 41.24... aliens. (a) Definition of international organization. “International organization” means: (1) Any public...)(27)(I), INTELSAT or any successor or separated entity thereof. (b) Aliens coming to international...

  20. 22 CFR 41.24 - International organization aliens.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 22 Foreign Relations 1 2013-04-01 2013-04-01 false International organization aliens. 41.24... aliens. (a) Definition of international organization. “International organization” means: (1) Any public...)(27)(I), INTELSAT or any successor or separated entity thereof. (b) Aliens coming to international...

  1. First derivative ratio spectrophotometric, HPTLC-densitometric, and HPLC determination of nicergoline in presence of its hydrolysis-induced degradation product.

    PubMed

    Ahmad, Abdel Kader S; Kawy, M Abdel; Nebsen, M

    2002-10-15

    Three methods are presented for the determination of Nicergoline in presence of its hydrolysis-induced degradation product. The first method was based on measurement of the first derivative of ratio spectra amplitude of Nicergoline at 291 nm. The second method was based on separation of Nicergoline from its degradation product followed by densitometric measurement of the spots at 287 nm. The separation was carried out on HPTLC silica gel F(254) plates, using methanol-ethyl acetate-glacial acetic acid (5:7:3, v/v/v) as mobile phase. The third method was based on high performance liquid chromatographic (HPLC) separation and determination of Nicergoline from its degradation product on a reversed phase, nucloesil C(18) column using a mobile phase of methanol-water-glacial acetic acid (80:20:0.1, v/v/v) with UV detection at 280 nm. Chlorpromazine hydrochloride was used as internal standard. Laboratory prepared mixtures containing different percentages of the degradation product were analysed by the proposed methods and satisfactory results were obtained. These methods have been successfully applied to the analysis of Nicergoline in Sermion tablets. The validities of these methods were ascertained by applying standard addition technique, the mean percentage recovery +/- R.S.D.% was found to be 99.47 +/- 0.752, 100.01 +/- 0.940, 99.75 +/- 0.740 for the first derivative of ratio spectra method, the HPTLC method and the HPLC method, respectively. The proposed methods were statistically compared with the manufacturer's HPLC method of analysis of Nicergoline and no significant difference was found with respect to both precision and accuracy. They have the advantage of being stability indicating. Therefore, they can be used for routine analysis of the drug in quality control laboratories. Copyright 2002 Elsevier Science B.V.

  2. 40 CFR 60.4231 - What emission standards must I meet if I am a manufacturer of stationary SI internal combustion...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... I am a manufacturer of stationary SI internal combustion engines or equipment containing such... Stationary Spark Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4231 What emission standards must I meet if I am a manufacturer of stationary SI internal combustion engines or...

  3. 40 CFR 60.4231 - What emission standards must I meet if I am a manufacturer of stationary SI internal combustion...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... I am a manufacturer of stationary SI internal combustion engines or equipment containing such... Stationary Spark Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4231 What emission standards must I meet if I am a manufacturer of stationary SI internal combustion engines or...

  4. 40 CFR 60.4231 - What emission standards must I meet if I am a manufacturer of stationary SI internal combustion...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... I am a manufacturer of stationary SI internal combustion engines or equipment containing such... Stationary Spark Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4231 What emission standards must I meet if I am a manufacturer of stationary SI internal combustion engines or...

  5. 40 CFR 60.4231 - What emission standards must I meet if I am a manufacturer of stationary SI internal combustion...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... I am a manufacturer of stationary SI internal combustion engines or equipment containing such... Stationary Spark Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4231 What emission standards must I meet if I am a manufacturer of stationary SI internal combustion engines or...

  6. 40 CFR 60.4231 - What emission standards must I meet if I am a manufacturer of stationary SI internal combustion...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... I am a manufacturer of stationary SI internal combustion engines or equipment containing such... Stationary Spark Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4231 What emission standards must I meet if I am a manufacturer of stationary SI internal combustion engines or...

  7. 25 CFR 542.42 - What are the minimum internal control standards for internal audit for Tier C gaming operations?

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... reconciliation process; (ii) Pull tabs, including but not limited to, statistical records, winner verification... 25 Indians 2 2010-04-01 2010-04-01 false What are the minimum internal control standards for... COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.42 What are...

  8. CMMI(Registered) for Acquisition, Version 1.3. CMMI-ACQ, V1.3

    DTIC Science & Technology

    2010-11-01

    and Software Engineering – System Life Cycle Processes [ ISO 2008b] ISO /IEC 27001 :2005 Information technology – Security techniques – Information...International Organization for Standardization and International Electrotechnical Commission. ISO /IEC 27001 Information Technology – Security Techniques...International Organization for Standardization/International Electrotechnical Commission ( ISO /IEC) body of standards. CMMs focus on improving processes

  9. An international Urogynecological association (IUGA)/international continence society (ICS) joint report on the terminology for the assessment of sexual health of women with pelvic floor dysfunction.

    PubMed

    Rogers, Rebecca G; Pauls, Rachel N; Thakar, Ranee; Morin, Melanie; Kuhn, Annette; Petri, Eckhard; Fatton, Brigitte; Whitmore, Kristene; Kingsberg, Sheryl A; Lee, Joseph

    2018-05-01

    The terminology in current use for sexual function and dysfunction in women with pelvic floor disorders lacks uniformity, which leads to uncertainty, confusion, and unintended ambiguity. The terminology for the sexual health of women with pelvic floor dysfunction needs to be collated in a clinically-based consensus report. This report combines the input of members of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA), and the International Continence Society (ICS), assisted at intervals by many external referees. Internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). Importantly, this report is not meant to replace, but rather complement current terminology used in other fields for female sexual health and to clarify terms specific to women with pelvic floor dysfunction. A clinically based terminology report for sexual health in women with pelvic floor dysfunction encompassing over 100 separate definitions, has been developed. Key aims have been to make the terminology interpretable by practitioners, trainees, and researchers in female pelvic floor dysfunction. Interval review (5-10 years) is anticipated to keep the document updated and as widely acceptable as possible. A consensus-based terminology report for female sexual health in women with pelvic floor dysfunction has been produced aimed at being a significant aid to clinical practice and a stimulus for research.

  10. An International Urogynecological Association (IUGA)/International Continence Society (ICS) joint report on the terminology for the conservative and nonpharmacological management of female pelvic floor dysfunction.

    PubMed

    Bo, Kari; Frawley, Helena C; Haylen, Bernard T; Abramov, Yoram; Almeida, Fernando G; Berghmans, Bary; Bortolini, Maria; Dumoulin, Chantale; Gomes, Mario; McClurg, Doreen; Meijlink, Jane; Shelly, Elizabeth; Trabuco, Emanuel; Walker, Carolina; Wells, Amanda

    2017-02-01

    There has been an increasing need for the terminology on the conservative management of female pelvic floor dysfunction to be collated in a clinically based consensus report. This Report combines the input of members and elected nominees of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA) and the International Continence Society (ICS), assisted at intervals by many external referees. An extensive process of nine rounds of internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). Before opening up for comments on the webpages of ICS and IUGA, five experts from physiotherapy, neurology, urology, urogynecology, and nursing were invited to comment on the paper. A Terminology Report on the conservative management of female pelvic floor dysfunction, encompassing over 200 separate definitions, has been developed. It is clinically based, with the most common symptoms, signs, assessments, diagnoses, and treatments defined. Clarity and ease of use have been key aims to make it interpretable by practitioners and trainees in all the different specialty groups involved in female pelvic floor dysfunction. Ongoing review is not only anticipated, but will be required to keep the document updated and as widely acceptable as possible. A consensus-based terminology report for the conservative management of female pelvic floor dysfunction has been produced, aimed at being a significant aid to clinical practice and a stimulus for research.

  11. An International Urogynecological Association (IUGA)/International Continence Society (ICS) joint report on the terminology for female anorectal dysfunction.

    PubMed

    Sultan, Abdul H; Monga, Ash; Lee, Joseph; Emmanuel, Anton; Norton, Christine; Santoro, Giulio; Hull, Tracy; Berghmans, Bary; Brody, Stuart; Haylen, Bernard T

    2017-01-01

    The terminology for anorectal dysfunction in women has long been in need of a specific clinically-based Consensus Report. This Report combines the input of members of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA) and the International Continence Society (ICS), assisted on Committee by experts in their fields to form a Joint IUGA/ICS Working Group on Female Anorectal Terminology. Appropriate core clinical categories and sub classifications were developed to give an alphanumeric coding to each definition. An extensive process of twenty rounds of internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). A Terminology Report for anorectal dysfunction, encompassing over 130 separate definitions, has been developed. It is clinically based with the most common diagnoses defined. Clarity and user-friendliness have been key aims to make it interpretable by practitioners and trainees in all the different specialty groups involved in female pelvic floor dysfunction. Female-specific anorectal investigations and imaging (ultrasound, radiology and MRI) has been included whilst appropriate figures have been included to supplement and help clarify the text. Interval review (5-10 years) is anticipated to keep the document updated and as widely acceptable as possible. A consensus-based Terminology Report for female anorectal dysfunction terminology has been produced aimed at being a significant aid to clinical practice and a stimulus for research.

  12. An International Urogynecological Association (IUGA)/International Continence Society (ICS) joint report on the terminology for the assessment of sexual health of women with pelvic floor dysfunction.

    PubMed

    Rogers, Rebecca G; Pauls, Rachel N; Thakar, Ranee; Morin, Melanie; Kuhn, Annette; Petri, Eckhard; Fatton, Brigitte; Whitmore, Kristene; Kinsberg, Sheryl; Lee, Joseph

    2018-04-01

    The terminology in current use for sexual function and dysfunction in women with pelvic floor disorders lacks uniformity, which leads to uncertainty, confusion, and unintended ambiguity. The terminology for the sexual health of women with pelvic floor dysfunction needs to be collated in a clinically-based consensus report. This report combines the input of members of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA), and the International Continence Society (ICS), assisted at intervals by many external referees. Internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). Importantly, this report is not meant to replace, but rather complement current terminology used in other fields for female sexual health and to clarify terms specific to women with pelvic floor dysfunction. A clinically based terminology report for sexual health in women with pelvic floor dysfunction encompassing over 100 separate definitions, has been developed. Key aims have been to make the terminology interpretable by practitioners, trainees, and researchers in female pelvic floor dysfunction. Interval review (5-10 years) is anticipated to keep the document updated and as widely acceptable as possible. A consensus-based terminology report for female sexual health in women with pelvic floor dysfunction has been produced aimed at being a significant aid to clinical practice and a stimulus for research. © 2018 Wiley Periodicals, Inc.

  13. Efforts to improve international migration statistics: a historical perspective.

    PubMed

    Kraly, E P; Gnanasekaran, K S

    1987-01-01

    During the past decade, the international statistical community has made several efforts to develop standards for the definition, collection and publication of statistics on international migration. This article surveys the history of official initiatives to standardize international migration statistics by reviewing the recommendations of the International Statistical Institute, International Labor Organization, and the UN, and reports a recently proposed agenda for moving toward comparability among national statistical systems. Heightening awareness of the benefits of exchange and creating motivation to implement international standards requires a 3-pronged effort from the international statistical community. 1st, it is essential to continue discussion about the significance of improvement, specifically standardization, of international migration statistics. The move from theory to practice in this area requires ongoing focus by migration statisticians so that conformity to international standards itself becomes a criterion by which national statistical practices are examined and assessed. 2nd, the countries should be provided with technical documentation to support and facilitate the implementation of the recommended statistical systems. Documentation should be developed with an understanding that conformity to international standards for migration and travel statistics must be achieved within existing national statistical programs. 3rd, the call for statistical research in this area requires more efforts by the community of migration statisticians, beginning with the mobilization of bilateral and multilateral resources to undertake the preceding list of activities.

  14. The standards process: X3 information processing systems

    NASA Technical Reports Server (NTRS)

    Emard, Jean-Paul

    1993-01-01

    The topics are presented in viewgraph form and include the following: International Organization for Standards (ISO); International Electrotechnical Committee (IEC); ISO/IEC Joint Technical Committee 1 (JTC-1); U.S. interface to JTC-1; ANSI; national organizations; U.S. standards development processes; national and international standards developing organizations; regional organizations; and X3 information processing systems.

  15. Validated LC–MS-MS Method for Multiresidual Analysis of 13 Illicit Phenethylamines in Amniotic Fluid

    PubMed Central

    Burrai, Lucia; Nieddu, Maria; Carta, Antonio; Trignano, Claudia; Sanna, Raimonda; Boatto, Gianpiero

    2016-01-01

    A multi-residue analytical method was developed for the determination in amniotic fluid (AF) of 13 illicit phenethylamines, including 12 compounds never investigated in this matrix before. Samples were subject to solid-phase extraction using; hydrophilic–lipophilic balance cartridges which gave good recoveries and low matrix effects on analysis of the extracts. The quantification was performed by liquid chromatography electrospray tandem mass spectrometry. The water–acetonitrile mobile phase containing 0.1% formic acid, used with a C18 reversed phase column, provided adequate separation, resolution and signal-to-noise ratio for the analytes and the internal standard. The final optimized method was validated according to international guidelines. A monitoring campaign to assess fetal exposure to these 13 substances of abuse has been performed on AF test samples obtained from pregnant women. All mothers (n = 194) reported no use of drugs of abuse during pregnancy, and this was confirmed by the analytical data. PMID:26755540

  16. Fast separation of enantiomers by capillary electrophoresis using a combination of two capillaries with different internal diameters.

    PubMed

    Šebestová, Andrea; Petr, Jan

    2017-12-01

    The combination of capillaries with different internal diameters was used to accelerate the separation of enantiomers in capillary electrophoresis. Separation of R,S-1,1'-binaphthalene-2,2'-diyl hydrogen phosphate using isopropyl derivative of cyclofructan 6 was studied as a model system. The best separation conditions included 500 mM sodium borate pH 9.5 with 60 mM concentration of the chiral selector. Separation lasted approx. 1.5 min using the combination of 50 and 100 μm id capillaries of 9.7 cm and 22.9 cm, respectively. It allowed approx. 12-fold acceleration in comparison to the traditional long-end separation mainly due to the higher electroosmotic flow generated in the connected capillaries. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. International Micrographics Standards: Report of the 1979 Paris Meeting of ISO/TC171.

    ERIC Educational Resources Information Center

    Heynen, Jeffrey

    1980-01-01

    Describes a meeting of the technical committee on micrographics of the International Organization for Standardization, and fcuses on the committee's work relating to the reproduction of library materials within the general context of international standards-making activities. (FM)

  18. Faculty Perspectives on International Accounting Topics.

    ERIC Educational Resources Information Center

    Smith, L. Murphy; Salter, Stephen B.

    1996-01-01

    A survey of 63 professors specializing in international accounting identified the following topics as most important to incorporate into the curriculum: (1) foreign currency translation; (2) international accounting standards; (3) comparative standards and harmonizing of accounting standards; (4) reporting and disclosure problems of multinational…

  19. Surfactant-free microemulsion electrokinetic chromatography (SF-MEEKC) with UV and MS detection - a novel approach for the separation and ESI-MS detection of neutral compounds.

    PubMed

    Mohorič, Urška; Beutner, Andrea; Krickl, Sebastian; Touraud, Didier; Kunz, Werner; Matysik, Frank-Michael

    2016-12-01

    Microemulsion electrokinetic chromatography (MEEKC) is a powerful tool to separate neutral species based on differences in their hydrophobic and hydrophilic properties. However, as a major drawback the conventionally used SDS based microemulsions are not compatible with electrospray ionization mass spectrometry (ESI-MS). In this work, a surfactant-free microemulsion (SFME) consisting of water, ethanol, and 1-octanol is used for surfactant-free microemulsion electrokinetic chromatography (SF-MEEKC). Ammonium acetate was added to the SFME enabling electrophoretic separations. The stability of SFMEs containing ammonium acetate was investigated using small-angle X-ray scattering and dynamic light scattering. A method for the separation of a model system of hydrophobic and hydrophilic neutral vitamins, namely the vitamins B 2 and D 3 , and the cationic vitamin B 1 was developed using UV/VIS detection. The influence of the ammonium acetate concentration on the separation performance was studied in detail. The method was characterized concerning reproducibility of migration times and peak areas and concerning the linearity of the calibration data. Furthermore, SF-MEEKC was coupled to ESI-MS investigating the compatibility between SFMEs and the ESI process. The signal intensities of ESI-MS measurements of the model analytes were comparable for SFMEs and aqueous systems. Finally, the vitamin D 3 content of a drug treating vitamin D 3 deficiency was determined by SF-MEEKC coupled to ESI-MS using 25-hydroxycholecalciferol as an internal standard. Graphical abstract The concept of surfactant-free microemulsion electrokinetic chromatography coupled to electrospray ionization mass spectrometry.

  20. Clinical curative effect of fuzi-cake-separated moxibustion for preventing dysuria after operation for lower limb fracture.

    PubMed

    Yue, Yan; Tao, Lijun; Fang, Jianqiao; Xie, Qi; He, Shaofeng; Huang, Chunxia; Yang, Xueming

    2014-10-01

    To assess the clinical curative effect of fuzi-cake-separated moxibustion at Zhongji (CV 3) and Guanyuan (CV 4) for preventing dysuria after internal fixation of lower limb fractures. Sixty patients conforming to the inclusion standards were randomly divided into a treatment group (n = 30) and a control group (n = 30). Fuzi-cake-separated moxibustion was performed at Guanyuan (CV 4) and Zhongji (CV 3), 20 min at a time, twice a day, for 3 days before operation in the treatment group. No fuzi-cake-separated moxibustion was performed in the control group. After treatment, the score for symptoms of first urination, urinary time, urinary volume, 24 h remaining urinary volume, incidence of uroschesis, and rate of controlling dysuria were compared to evaluate the curative effect of preventing post-operative dysuria. The score for symptoms of first urination, 24 h remaining urinary volume (maximum 120 mL vs 250 ml, and less than 10 ml in 24 cases vs 15 cases), and the rate of controlling dysuria (83.34% vs 30%) were significantly better (P < 0.05, P < 0.05, and P < 0.001, respectively) in the treatment compared with the control group. There was no statistical difference (P > 0.05) between the two groups in first post-operative urinary time, urinary volume, or incidence of 24 h uroschesis. Fuzi-cake-separated moxibustion at Zhongji (CV 3) and Guanyuan (CV 4) can better prevent post-operative dysuria, effectively promote the functional restoration of the urinary bladder, and control the incidence of post-operative dysuria.

  1. Specific features of the cathodoluminescence spectra of AlInGaN QWs, caused by the influence of phase separation and internal electric fields

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

    Kuznetsova, Ya. V., E-mail: yana@mail.ioffe.ru; Jmerik, V. N.; Nechaev, D. V.

    2016-07-15

    The specific features of the cathodoluminescence (CL) spectra in AlInGaN heterostructures, caused by the influence of phase separation and internal electric fields, observed at varied CL excitation density, are studied. It is shown that the evolution of the CL spectrum and the variation in the spectral position of emission lines of nanoscale layers with current density in the primary electron beam makes it possible to identify the occurrence of phase separation in the layer and, in the absence of this separation, to estimate the electric-field strength in the active region of the structure.

  2. Standard requirements for GCP-compliant data management in multinational clinical trials.

    PubMed

    Ohmann, Christian; Kuchinke, Wolfgang; Canham, Steve; Lauritsen, Jens; Salas, Nader; Schade-Brittinger, Carmen; Wittenberg, Michael; McPherson, Gladys; McCourt, John; Gueyffier, Francois; Lorimer, Andrea; Torres, Ferràn

    2011-03-22

    A recent survey has shown that data management in clinical trials performed by academic trial units still faces many difficulties (e.g. heterogeneity of software products, deficits in quality management, limited human and financial resources and the complexity of running a local computer centre). Unfortunately, no specific, practical and open standard for both GCP-compliant data management and the underlying IT-infrastructure is available to improve the situation. For that reason the "Working Group on Data Centres" of the European Clinical Research Infrastructures Network (ECRIN) has developed a standard specifying the requirements for high quality GCP-compliant data management in multinational clinical trials. International, European and national regulations and guidelines relevant to GCP, data security and IT infrastructures, as well as ECRIN documents produced previously, were evaluated to provide a starting point for the development of standard requirements. The requirements were produced by expert consensus of the ECRIN Working group on Data Centres, using a structured and standardised process. The requirements were divided into two main parts: an IT part covering standards for the underlying IT infrastructure and computer systems in general, and a Data Management (DM) part covering requirements for data management applications in clinical trials. The standard developed includes 115 IT requirements, split into 15 separate sections, 107 DM requirements (in 12 sections) and 13 other requirements (2 sections). Sections IT01 to IT05 deal with the basic IT infrastructure while IT06 and IT07 cover validation and local software development. IT08 to IT015 concern the aspects of IT systems that directly support clinical trial management. Sections DM01 to DM03 cover the implementation of a specific clinical data management application, i.e. for a specific trial, whilst DM04 to DM12 address the data management of trials across the unit. Section IN01 is dedicated to international aspects and ST01 to the competence of a trials unit's staff. The standard is intended to provide an open and widely used set of requirements for GCP-compliant data management, particularly in academic trial units. It is the intention that ECRIN will use these requirements as the basis for the certification of ECRIN data centres.

  3. 25 CFR 542.22 - What are the minimum internal control standards for internal audit for Tier A gaming operations?

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... but not limited to, bingo card control, payout procedures, and cash reconciliation process; (ii) Pull... 25 Indians 2 2010-04-01 2010-04-01 false What are the minimum internal control standards for... COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.22 What are...

  4. 25 CFR 542.32 - What are the minimum internal control standards for internal audit for Tier B gaming operations?

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... but not limited to, bingo card control, payout procedures, and cash reconciliation process; (ii) Pull... 25 Indians 2 2010-04-01 2010-04-01 false What are the minimum internal control standards for... COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.32 What are...

  5. Standardized Cardiovascular Data for Clinical Research, Registries, and Patient Care

    PubMed Central

    Anderson, H. Vernon; Weintraub, William S.; Radford, Martha J.; Kremers, Mark S.; Roe, Matthew T.; Shaw, Richard E.; Pinchotti, Dana M.; Tcheng, James E.

    2013-01-01

    Relatively little attention has been focused on standardization of data exchange in clinical research studies and patient care activities. Both are usually managed locally using separate and generally incompatible data systems at individual hospitals or clinics. In the past decade there have been nascent efforts to create data standards for clinical research and patient care data, and to some extent these are helpful in providing a degree of uniformity. Nevertheless these data standards generally have not been converted into accepted computer-based language structures that could permit reliable data exchange across computer networks. The National Cardiovascular Research Infrastructure (NCRI) project was initiated with a major objective of creating a model framework for standard data exchange in all clinical research, clinical registry, and patient care environments, including all electronic health records. The goal is complete syntactic and semantic interoperability. A Data Standards Workgroup was established to create or identify and then harmonize clinical definitions for a base set of standardized cardiovascular data elements that could be used in this network infrastructure. Recognizing the need for continuity with prior efforts, the Workgroup examined existing data standards sources. A basic set of 353 elements was selected. The NCRI staff then collaborated with the two major technical standards organizations in healthcare, the Clinical Data Interchange Standards Consortium and Health Level 7 International, as well as with staff from the National Cancer Institute Enterprise Vocabulary Services. Modeling and mapping were performed to represent (instantiate) the data elements in appropriate technical computer language structures for endorsement as an accepted data standard for public access and use. Fully implemented, these elements will facilitate clinical research, registry reporting, administrative reporting and regulatory compliance, and patient care. PMID:23500238

  6. Chapter 23: International Standard reagents for harmonization of HPV serology and DNA assays--an update.

    PubMed

    Pagliusi, Sonia R; Dillner, Joakim; Pawlita, Michael; Quint, Wim G V; Wheeler, Cosette M; Ferguson, M

    2006-08-31

    International reference materials such as International Standard reagents facilitate quality assurance of essential biopharmaceutical products and related in vitro diagnostic tests. Standardization of antibody and DNA measurements and harmonization of laboratory procedures are key to the success of cancer prevention strategies through screening methods as well as for development and implementation of vaccination against the human papillomavirus (HPV). The WHO supported the preparation and initial analysis of a panel of candidate serological and DNA reference reagents aimed at facilitating inter-laboratory comparisons and detection of HPV worldwide. Two international collaborative studies assessed the performance of various HPV antibody and HPV-DNA detection assays and examined the feasibility of generating HPV antibody and DNA standard reagents. These studies showed that improvement in performance and comparability of assays is urgently needed and that the use of the same International Standard reference reagent could significantly improve performance and comparability. It is hoped that the establishment of International Units and International Standards for HPV antibody and DNA analysis will be pursued with high priority.

  7. Housekeeping genes as internal standards: use and limits.

    PubMed

    Thellin, O; Zorzi, W; Lakaye, B; De Borman, B; Coumans, B; Hennen, G; Grisar, T; Igout, A; Heinen, E

    1999-10-08

    Quantitative studies are commonly realised in the biomedical research to compare RNA expression in different experimental or clinical conditions. These quantifications are performed through their comparison to the expression of the housekeeping gene transcripts like glyceraldehyde-3-phosphate dehydrogenase (G3PDH), albumin, actins, tubulins, cyclophilin, hypoxantine phsophoribosyltransferase (HRPT), L32. 28S, and 18S rRNAs are also used as internal standards. In this paper, it is recalled that the commonly used internal standards can quantitatively vary in response to various factors. Possible variations are illustrated using three experimental examples. Preferred types of internal standards are then proposed for each of these samples and thereafter the general procedure concerning the choice of an internal standard and the way to manage its uses are discussed.

  8. [Internalization disorders in children with asthma].

    PubMed

    Carrera-Bojorges, Xûchitl Beatriz; Pérez-Romero, Luis Francisco; Trujillo-Garcìa, José Ubaldo; Jiménez-Sandoval, Jaime Omar; Machorro-Muñoz, Olga Stephanie

    2013-01-01

    The presence of asthma may increase the risk for internalizing disorders such as major depression and anxiety. To determine if the diagnosis of asthma in children is associated with other internalizing disorders such as panic disorder, social phobia, separation anxiety, and total anxiety. In this analytical, descriptive and comparative cross sectional study, 144 asthmatic and 144 nonasthmatic patients, with ages between 8 and 17 years, were included. We used the GINA asthma diagnostic criteria. We applied the Hospital Anxiety and Depression Scale for diagnosis of internalizing disorders. Asthmatic children had a significant association with panic disorder P 0.001, RP 2.7; with social phobia P 0.026, RP 2.5; with separation anxiety P 0.002, RP 3.3; and with total anxiety P 0.017, RP 2.3. Nonasthmatic children did not have these associations. Asthma severity was intermittent in 36 cases (12.5%), mild persistent in 86 (29.9%) cases, and moderate persistent in 22 (7.6%) cases. We observed no statistically significant relationship between the severity of asthma and the diagnosis of an internalization disorder. We observed a meaningful association between asthma and internalizing disorders such as panic disorder, social phobia, separation anxiety and total anxiety in children.

  9. Issues concerning international comparison of free-field calibrations of acoustical standards

    NASA Astrophysics Data System (ADS)

    Nedzelnitsky, Victor

    2002-11-01

    Primary free-field calibrations of laboratory standard microphones by the reciprocity method establish these microphones as reference standard devices for calibrating working standard microphones, other measuring microphones, and practical instruments such as sound level meters and personal sound exposure meters (noise dosimeters). These primary, secondary, and other calibrations are indispensable to the support of regulatory requirements, standards, and product characterization and quality control procedures important for industry, commerce, health, and safety. International Electrotechnical Commission (IEC) Technical Committee 29 Electroacoustics produces international documentary standards, including standards for primary and secondary free-field calibration and measurement procedures and their critically important application to practical instruments. This paper addresses some issues concerning calibrations, standards activities, and the international key comparison of primary free-field calibrations of IEC-type LS2 laboratory standard microphones that is being planned by the Consultative Committee for Acoustics, Ultrasound, and Vibration (CCAUV) of the International Committee for Weights and Measures (CIPM). This comparison will include free-field calibrations by the reciprocity method at participating major national metrology laboratories throughout the world.

  10. International standards in mitigating trade risks.

    PubMed

    Thiermann, A B

    2011-04-01

    This paper describes the role of the World Organisation for Animal Health (OIE), as a science-based and democratic standard-setting organisation that provides guidance on preventing the spread of animal diseases, including zoonoses, in international trade. The World Trade Organization is identified as the international institution with the legal power to encourage adherence to international standards and mediate trade disputes. The importance of assuring good governance and the credibility of national Veterinary Services through a process of official certification is identified as an essential component in the safety of trade. Private-public partnerships and the evolution of responsibilities are also identified as essential for the implementation of health guarantees such as compartmentalisation. The rapid emergence of private standards is described as a potential complement to the implementation of sanitary standards, as long as they are applied globally and in support of the OIE standards. Ultimately, the biggest challenge is for the international community to create the incentives and generate the political will for fair trade and for the universal recognition and application of the established international sanitary standards.

  11. An International Urogynecological Association (IUGA)/International Continence Society (ICS) joint report on the terminology for the conservative and nonpharmacological management of female pelvic floor dysfunction.

    PubMed

    Bo, Kari; Frawley, Helena C; Haylen, Bernard T; Abramov, Yoram; Almeida, Fernando G; Berghmans, Bary; Bortolini, Maria; Dumoulin, Chantale; Gomes, Mario; McClurg, Doreen; Meijlink, Jane; Shelly, Elizabeth; Trabuco, Emanuel; Walker, Carolina; Wells, Amanda

    2017-02-01

    Introduction and hypothesis There has been an increasing need for the terminology on the conservative management of female pelvic floor dysfunction to be collated in a clinically based consensus report. Methods This Report combines the input of members and elected nominees of the Standardization and Terminology Committees of two International Organizations, the International Urogynecological Association (IUGA) and the International Continence Society (ICS), assisted at intervals by many external referees. An extensive process of nine rounds of internal and external review was developed to exhaustively examine each definition, with decision-making by collective opinion (consensus). Before opening up for comments on the webpages of ICS and IUGA, five experts from physiotherapy, neurology, urology, urogynecology, and nursing were invited to comment on the paper. Results A Terminology Report on the conservative management of female pelvic floor dysfunction, encompassing over 200 separate definitions, has been developed. It is clinically based, with the most common symptoms, signs, assessments, diagnoses, and treatments defined. Clarity and ease of use have been key aims to make it interpretable by practitioners and trainees in all the different specialty groups involved in female pelvic floor dysfunction. Ongoing review is not only anticipated, but will be required to keep the document updated and as widely acceptable as possible. Conclusion A consensus-based terminology report for the conservative management of female pelvic floor dysfunction has been produced, aimed at being a significant aid to clinical practice and a stimulus for research. © 2016 Wiley Periodicals, Inc., and The International Urogynecological Association.

  12. 26 CFR 1.663(c)-1 - Separate shares treated as separate trusts or as separate estates; in general.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... of applicable law in situations in which a single trust (or estate) instrument creates not one but... 26 Internal Revenue 8 2010-04-01 2010-04-01 false Separate shares treated as separate trusts or as..., DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES Estates and Trusts Which May...

  13. Use of exhaust gas as sweep flow to enhance air separation membrane performance

    DOEpatents

    Dutart, Charles H.; Choi, Cathy Y.

    2003-01-01

    An intake air separation system for an internal combustion engine is provided with purge gas or sweep flow on the permeate side of separation membranes in the air separation device. Exhaust gas from the engine is used as a purge gas flow, to increase oxygen flux in the separation device without increasing the nitrogen flux.

  14. 26 CFR 1.414(r)-9 - Separate application of section 401(a)(26).

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ....414(r)-9 Section 1.414(r)-9 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-9 Separate application of section 401(a)(26). (a) General rule. If an employer is treated... with § 1.414(r)-1(b) for a testing year, the requirements of section 401(a)(26) must be applied...

  15. 26 CFR 1.414(r)-9 - Separate application of section 401(a)(26).

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ....414(r)-9 Section 1.414(r)-9 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY (CONTINUED) INCOME TAX (CONTINUED) INCOME TAXES Pension, Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-9... qualified separate lines of business for purposes of section 401(a)(26) in accordance with § 1.414(r)-1(b...

  16. 26 CFR 1.414(r)-4 - Qualified separate line of business-fifty-employee and notice requirements.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...-employee and notice requirements. 1.414(r)-4 Section 1.414(r)-4 Internal Revenue INTERNAL REVENUE SERVICE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-4 Qualified separate line of business—fifty-employee and... line of business (as determined under § 1.414(r)-3) satisfies the 50-employee and notice requirements...

  17. 26 CFR 1.414(r)-5 - Qualified separate line of business-administrative scrutiny requirement-safe harbors.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...-administrative scrutiny requirement-safe harbors. 1.414(r)-5 Section 1.414(r)-5 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-5 Qualified separate line of business—administrative...(r)-3 satisfies the administrative scrutiny requirement of § 1.414(r)-1(b)(2)(iv)(D) for a testing...

  18. 26 CFR 1.414(r)-5 - Qualified separate line of business-administrative scrutiny requirement-safe harbors.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ...-administrative scrutiny requirement-safe harbors. 1.414(r)-5 Section 1.414(r)-5 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-5 Qualified separate line of business—administrative...(r)-3 satisfies the administrative scrutiny requirement of § 1.414(r)-1(b)(2)(iv)(D) for a testing...

  19. 26 CFR 1.414(r)-4 - Qualified separate line of business-fifty-employee and notice requirements.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ...-employee and notice requirements. 1.414(r)-4 Section 1.414(r)-4 Internal Revenue INTERNAL REVENUE SERVICE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-4 Qualified separate line of business—fifty-employee and... line of business (as determined under § 1.414(r)-3) satisfies the 50-employee and notice requirements...

  20. 26 CFR 1.414(r)-5 - Qualified separate line of business-administrative scrutiny requirement-safe harbors.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...-administrative scrutiny requirement-safe harbors. 1.414(r)-5 Section 1.414(r)-5 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-5 Qualified separate line of business—administrative...(r)-3 satisfies the administrative scrutiny requirement of § 1.414(r)-1(b)(2)(iv)(D) for a testing...

  1. 26 CFR 1.414(r)-9 - Separate application of section 401(a)(26).

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ....414(r)-9 Section 1.414(r)-9 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-9 Separate application of section 401(a)(26). (a) General rule. If an employer is treated... with § 1.414(r)-1(b) for a testing year, the requirements of section 401(a)(26) must be applied...

  2. 26 CFR 1.414(r)-4 - Qualified separate line of business-fifty-employee and notice requirements.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...-employee and notice requirements. 1.414(r)-4 Section 1.414(r)-4 Internal Revenue INTERNAL REVENUE SERVICE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-4 Qualified separate line of business—fifty-employee and... line of business (as determined under § 1.414(r)-3) satisfies the 50-employee and notice requirements...

  3. 26 CFR 1.414(r)-5 - Qualified separate line of business-administrative scrutiny requirement-safe harbors.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ...-administrative scrutiny requirement-safe harbors. 1.414(r)-5 Section 1.414(r)-5 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-5 Qualified separate line of business—administrative...(r)-3 satisfies the administrative scrutiny requirement of § 1.414(r)-1(b)(2)(iv)(D) for a testing...

  4. 26 CFR 1.414(r)-9 - Separate application of section 401(a)(26).

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ....414(r)-9 Section 1.414(r)-9 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-9 Separate application of section 401(a)(26). (a) General rule. If an employer is treated... with § 1.414(r)-1(b) for a testing year, the requirements of section 401(a)(26) must be applied...

  5. 26 CFR 1.414(r)-9 - Separate application of section 401(a)(26).

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ...(r)-9 Section 1.414(r)-9 Internal Revenue INTERNAL REVENUE SERVICE, DEPARTMENT OF THE TREASURY.... § 1.414(r)-9 Separate application of section 401(a)(26). (a) General rule. If an employer is treated... with § 1.414(r)-1(b) for a testing year, the requirements of section 401(a)(26) must be applied...

  6. 26 CFR 1.414(r)-4 - Qualified separate line of business-fifty-employee and notice requirements.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ...-employee and notice requirements. 1.414(r)-4 Section 1.414(r)-4 Internal Revenue INTERNAL REVENUE SERVICE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-4 Qualified separate line of business—fifty-employee and... line of business (as determined under § 1.414(r)-3) satisfies the 50-employee and notice requirements...

  7. 40 CFR 60.4232 - How long must my engines meet the emission standards if I am a manufacturer of stationary SI...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... emission standards if I am a manufacturer of stationary SI internal combustion engines? 60.4232 Section 60... Internal Combustion Engines Emission Standards for Manufacturers § 60.4232 How long must my engines meet the emission standards if I am a manufacturer of stationary SI internal combustion engines? Engines...

  8. 40 CFR 60.4232 - How long must my engines meet the emission standards if I am a manufacturer of stationary SI...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... emission standards if I am a manufacturer of stationary SI internal combustion engines? 60.4232 Section 60... Internal Combustion Engines Emission Standards for Manufacturers § 60.4232 How long must my engines meet the emission standards if I am a manufacturer of stationary SI internal combustion engines? Engines...

  9. 40 CFR 60.4232 - How long must my engines meet the emission standards if I am a manufacturer of stationary SI...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... emission standards if I am a manufacturer of stationary SI internal combustion engines? 60.4232 Section 60... Internal Combustion Engines Emission Standards for Manufacturers § 60.4232 How long must my engines meet the emission standards if I am a manufacturer of stationary SI internal combustion engines? Engines...

  10. 40 CFR 60.4203 - How long must my engines meet the emission standards if I am a stationary CI internal combustion...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... emission standards if I am a stationary CI internal combustion engine manufacturer? 60.4203 Section 60.4203... Combustion Engines Emission Standards for Manufacturers § 60.4203 How long must my engines meet the emission standards if I am a stationary CI internal combustion engine manufacturer? Engines manufactured by...

  11. 40 CFR 60.4203 - How long must my engines meet the emission standards if I am a stationary CI internal combustion...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... emission standards if I am a stationary CI internal combustion engine manufacturer? 60.4203 Section 60.4203... Combustion Engines Emission Standards for Manufacturers § 60.4203 How long must my engines meet the emission standards if I am a stationary CI internal combustion engine manufacturer? Engines manufactured by...

  12. 40 CFR 60.4203 - How long must my engines meet the emission standards if I am a manufacturer of stationary CI...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... emission standards if I am a manufacturer of stationary CI internal combustion engines? 60.4203 Section 60... Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4203 How long must my engines meet the emission standards if I am a manufacturer of stationary CI internal combustion engines...

  13. 40 CFR 60.4203 - How long must my engines meet the emission standards if I am a manufacturer of stationary CI...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... emission standards if I am a manufacturer of stationary CI internal combustion engines? 60.4203 Section 60... Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4203 How long must my engines meet the emission standards if I am a manufacturer of stationary CI internal combustion engines...

  14. 40 CFR 60.4232 - How long must my engines meet the emission standards if I am a manufacturer of stationary SI...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... emission standards if I am a manufacturer of stationary SI internal combustion engines? 60.4232 Section 60... Internal Combustion Engines Emission Standards for Manufacturers § 60.4232 How long must my engines meet the emission standards if I am a manufacturer of stationary SI internal combustion engines? Engines...

  15. 40 CFR 60.4203 - How long must my engines meet the emission standards if I am a manufacturer of stationary CI...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... emission standards if I am a manufacturer of stationary CI internal combustion engines? 60.4203 Section 60... Ignition Internal Combustion Engines Emission Standards for Manufacturers § 60.4203 How long must my engines meet the emission standards if I am a manufacturer of stationary CI internal combustion engines...

  16. 40 CFR 60.4232 - How long must my engines meet the emission standards if I am a manufacturer of stationary SI...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... emission standards if I am a manufacturer of stationary SI internal combustion engines? 60.4232 Section 60... Internal Combustion Engines Emission Standards for Manufacturers § 60.4232 How long must my engines meet the emission standards if I am a manufacturer of stationary SI internal combustion engines? Engines...

  17. Report of the Task Force on Testing Standards (TFTS) to the International Language Testing Association (ILTA).

    ERIC Educational Resources Information Center

    International Language Testing Association.

    The Task Force on Testing Standards (TFTS) of the International Language Testing Association was charged to produce a report of an international survey of language assessment standards, to provide for exchange of information on standards and for development of a code of practice. Contact with individuals in both language testing and the broader…

  18. Development and validation of a high throughput assay for the quantification of multiple green tea-derived catechins in human plasma.

    PubMed

    Mawson, Deborah H; Jeffrey, Keon L; Teale, Philip; Grace, Philip B

    2018-06-19

    A rapid, accurate and robust method for the determination of catechin (C), epicatechin (EC), gallocatechin (GC), epigallocatechin (EGC), catechin gallate (Cg), epicatechin gallate (ECg), gallocatechin gallate (GCg) and epigallocatechin gallate (EGCg) concentrations in human plasma has been developed. The method utilises protein precipitation following enzyme hydrolysis, with chromatographic separation and detection using reversed-phase liquid chromatography - tandem mass spectrometry (LC-MS/MS). Traditional issues such as lengthy chromatographic run times, sample and extract stability, and lack of suitable internal standards have been addressed. The method has been evaluated using a comprehensive validation procedure, confirming linearity over appropriate concentration ranges, and inter/intra batch precision and accuracies within suitable thresholds (precisions within 13.8% and accuracies within 12.4%). Recoveries of analytes were found to be consistent between different matrix samples, compensated for using suitable internal markers and within the performance of the instrumentation used. Similarly, chromatographic interferences have been corrected using the internal markers selected. Stability of all analytes in matrix is demonstrated over 32 days and throughout extraction conditions. This method is suitable for high throughput sample analysis studies. This article is protected by copyright. All rights reserved.

  19. 40 CFR 63.1042 - Standards-Separator fixed roof.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 10 2010-07-01 2010-07-01 false Standards-Separator fixed roof. 63.1042 Section 63.1042 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR PROGRAMS..., ignitable, explosive, reactive, or hazardous materials. (3) Opening of a safety device, as defined in § 63...

  20. Setting the Standards.

    ERIC Educational Resources Information Center

    Ryan, Ellen

    1994-01-01

    New Council for Advancement and Support of Education (CASE) standards for college and university fund raising establish three key rules for campaign reporting: (1) separation of gifts for featured and unspecified objectives; (2) separation of current from deferred gifts; and (3) disclosure of both face value and discounted present value of…

  1. 46 CFR 108.503 - Relationship to international standards.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 46 Shipping 4 2010-10-01 2010-10-01 false Relationship to international standards. 108.503 Section 108.503 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) A-MOBILE OFFSHORE DRILLING UNITS DESIGN AND EQUIPMENT Lifesaving Equipment § 108.503 Relationship to international standards. For...

  2. Standardizing Naming Conventions in Radiation Oncology

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

    Santanam, Lakshmi; Hurkmans, Coen; Mutic, Sasa

    2012-07-15

    Purpose: The aim of this study was to report on the development of a standardized target and organ-at-risk naming convention for use in radiation therapy and to present the nomenclature for structure naming for interinstitutional data sharing, clinical trial repositories, integrated multi-institutional collaborative databases, and quality control centers. This taxonomy should also enable improved plan benchmarking between clinical institutions and vendors and facilitation of automated treatment plan quality control. Materials and Methods: The Advanced Technology Consortium, Washington University in St. Louis, Radiation Therapy Oncology Group, Dutch Radiation Oncology Society, and the Clinical Trials RT QA Harmonization Group collaborated in creatingmore » this new naming convention. The International Commission on Radiation Units and Measurements guidelines have been used to create standardized nomenclature for target volumes (clinical target volume, internal target volume, planning target volume, etc.), organs at risk, and planning organ-at-risk volumes in radiation therapy. The nomenclature also includes rules for specifying laterality and margins for various structures. The naming rules distinguish tumor and nodal planning target volumes, with correspondence to their respective tumor/nodal clinical target volumes. It also provides rules for basic structure naming, as well as an option for more detailed names. Names of nonstandard structures used mainly for plan optimization or evaluation (rings, islands of dose avoidance, islands where additional dose is needed [dose painting]) are identified separately. Results: In addition to its use in 16 ongoing Radiation Therapy Oncology Group advanced technology clinical trial protocols and several new European Organization for Research and Treatment of Cancer protocols, a pilot version of this naming convention has been evaluated using patient data sets with varying treatment sites. All structures in these data sets were satisfactorily identified using this nomenclature. Conclusions: Use of standardized naming conventions is important to facilitate comparison of dosimetry across patient datasets. The guidelines presented here will facilitate international acceptance across a wide range of efforts, including groups organizing clinical trials, Radiation Oncology Institute, Dutch Radiation Oncology Society, Integrating the Healthcare Enterprise, Radiation Oncology domain (IHE-RO), and Digital Imaging and Communication in Medicine (DICOM).« less

  3. Crowdsourced Mapping - Letting Amateurs Into the Temple?

    NASA Astrophysics Data System (ADS)

    McCullagh, M.; Jackson, M.

    2013-05-01

    The rise of crowdsourced mapping data is well documented and attempts to integrate such information within existing or potential NSDIs [National Spatial Data Infrastructures] are increasingly being examined. The results of these experiments, however, have been mixed and have left many researchers uncertain and unclear of the benefits of integration and of solutions to problems of use for such combined and potentially synergistic mapping tools. This paper reviews the development of the crowdsource mapping movement and discusses the applications that have been developed and some of the successes achieved thus far. It also describes the problems of integration and ways of estimating success, based partly on a number of on-going studies at the University of Nottingham that look at different aspects of the integration problem: iterative improvement of crowdsource data quality, comparison between crowdsourced data and prior knowledge and models, development of trust in such data, and the alignment of variant ontologies. Questions of quality arise, particularly when crowdsource data are combined with pre-existing NSDI data. The latter is usually stable, meets international standards and often provides national coverage for use at a variety of scales. The former is often partial, without defined quality standards, patchy in coverage, but frequently addresses themes very important to some grass roots group and often to society as a whole. This group might be of regional, national, or international importance that needs a mapping facility to express its views, and therefore should combine with local NSDI initiatives to provide valid mapping. Will both groups use ISO (International Organisation for Standardisation) and OGC (Open Geospatial Consortium) standards? Or might some extension or relaxation be required to accommodate the mostly less rigorous crowdsourced data? So, can crowdsourced data ever be safely and successfully merged into an NSDI? Should it be simply a separate mapping layer? Is full integration possible providing quality standards are fully met, and methods of defining levels of quality agreed? Frequently crowdsourced data sets are anarchic in composition, and based on new and sometimes unproved technologies. Can an NSDI exhibit the necessary flexibility and speed to deal with such rapid technological and societal change?

  4. Analytical method for the identification and assay of 12 phthalates in cosmetic products: application of the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques".

    PubMed

    Gimeno, Pascal; Maggio, Annie-Françoise; Bousquet, Claudine; Quoirez, Audrey; Civade, Corinne; Bonnet, Pierre-Antoine

    2012-08-31

    Esters of phthalic acid, more commonly named phthalates, may be present in cosmetic products as ingredients or contaminants. Their presence as contaminant can be due to the manufacturing process, to raw materials used or to the migration of phthalates from packaging when plastic (polyvinyl chloride--PVC) is used. 8 phthalates (DBP, DEHP, BBP, DMEP, DnPP, DiPP, DPP, and DiBP), classified H360 or H361, are forbidden in cosmetics according to the European regulation on cosmetics 1223/2009. A GC/MS method was developed for the assay of 12 phthalates in cosmetics, including the 8 phthalates regulated. Analyses are carried out on a GC/MS system with electron impact ionization mode (EI). The separation of phthalates is obtained on a cross-linked 5%-phenyl/95%-dimethylpolysiloxane capillary column 30 m × 0.25 mm (i.d.) × 0.25 mm film thickness using a temperature gradient. Phthalate quantification is performed by external calibration using an internal standard. Validation elements obtained on standard solutions, highlight a satisfactory system conformity (resolution>1.5), a common quantification limit at 0.25 ng injected, an acceptable linearity between 0.5 μg mL⁻¹ and 5.0 μg mL⁻¹ as well as a precision and an accuracy in agreement with in-house specifications. Cosmetic samples ready for analytical injection are analyzed after a dilution in ethanol whereas more complex cosmetic matrices, like milks and creams, are assayed after a liquid/liquid extraction using ter-butyl methyl ether (TBME). Depending on the type of cosmetics analyzed, the common limits of quantification for the 12 phthalates were set at 0.5 or 2.5 μg g⁻¹. All samples were assayed using the analytical approach described in the ISO 12787 international standard "Cosmetics-Analytical methods-Validation criteria for analytical results using chromatographic techniques". This analytical protocol is particularly adapted when it is not possible to make reconstituted sample matrices. Copyright © 2012 Elsevier B.V. All rights reserved.

  5. Third International Standard for Posterior Pituitary

    PubMed Central

    Bangham, D. R.; Mussett, Marjorie V.

    1958-01-01

    In October 1955, stocks of the Second International Standard for Posterior Pituitary were running low and the Department of Biological Standards of the National Institute for Medical Research, London, was asked to proceed with the arrangements for an international collaborative assay of material for the Third Standard. A single 142-g batch of posterior-pituitary-lobe powder was obtained and distributed in ampoules, in approximately 30-mg quantities. Samples were sent to 19 laboratories in 10 countries. In all, 185 assays were carried out, 122 for oxytocic activity, 53 for vasopressor activity and 10 for antidiuretic activity. On the basis of the results, which were analysed statistically at the National Institute for Medical Research, it was agreed that the potency of the Third Standard (re-named International Standard for Oxytocic, Vasopressor and Antidiuretic Substances in 1956, in view of the recent synthesis of oxytocin and vasopressin) should be expressed as 2.0 International Units per milligram. The International Unit therefore remains unchanged as 0.5 mg of the dry powder. PMID:13585079

  6. Miniaturised electrically actuated high pressure injection valve for portable capillary liquid chromatography.

    PubMed

    Li, Yan; Pace, Kirsten; Nesterenko, Pavel N; Paull, Brett; Stanley, Roger; Macka, Mirek

    2018-04-01

    A miniaturised high pressure 6-port injection valve has been designed and evaluated for its performance in order to facilitate the development of portable capillary high performance liquid chromatography (HPLC). The electrically actuated valve features a very small size (65 × 19 × 19mm) and light weight (33g), and therefore can be easily integrated in a miniaturised modular capillary LC system suited for portable field analysis. The internal volume of the injection valve was determined as 98 nL. The novel conical shape of the stator and rotor and the spring-loaded rotor performed well up to 32MPa (4641psi), the maximum operating pressure investigated. Suitability for application was demonstrated using a miniaturised capillary LC system applied to the chromatographic separation of a mixture of biogenic amines and common cations. The RSD (relative standard deviation) values of retention times and peak areas of 6 successive runs were 0.5-0.7% and 1.8-2.8% for the separation of biogenic amines, respectively, and 0.1-0.2% and 2.1-3.0% for the separation of cations, respectively. This performance was comparable with bench-top HPLC systems thus demonstrating the applicability of the valve for use in portable and miniaturised capillary HPLC systems. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Quantitative determination of p-aminosalicylic acid and its degradation product m-aminophenol in pellets by ion-pair high-performance liquid chromatography applying the monolithic Chromolith Speedrod RP-18e column.

    PubMed

    Vasbinder, E; Van der Weken, G; Vander Heyden, Y; Baeyens, W R G; Debunne, A; Remon, J P; García-Campaña, A M

    2004-01-01

    An ion-pair high performance liquid chromatographic method was developed for the simultaneous determination of p-aminosalicylic acid (PAS) and its degradation product m-aminophenol (MAP) in a newly developed multiparticular drug delivery system. Owing to the concentration differences of PAS and MAP, acetanilide and sulfanilic acid were used as internal standards, respectively. The separation was performed on a Chromolith SpeedROD RP-18e column, a new packing material consisting of monolithic rods of highly porous silica. The mobile phase composition was of 20 mm phosphate buffer, 20 mm tetrabutylammonium hydrogen sulphate and 16% (v/v) methanol adjusted to pH 6.8, at a flow-rate of 1.0 mL/min, resulting in a run-time of about 6 min. Detection was by UV at 233 nm. The method was validated and proved to be useful for stability testing of the new dosage form. Separation efficiency was compared between the new packing material Chromolith SpeedROD RP-18e and the conventional reversed-phase cartridge LiChroCART 125-4 (5 microm). A robustness test was carried out on both columns and different separation parameters (retention, resolution, run time, temperature) were determined. Copyright 2004 John Wiley & Sons, Ltd.

  8. Rapid determination of piracetam in human plasma and cerebrospinal fluid by micellar electrokinetic chromatography with sample direct injection.

    PubMed

    Yeh, Hsin-Hua; Yang, Yuan-Han; Ko, Ju-Yun; Chen, Su-Hwei

    2006-07-07

    A simple micellar electrokinetic chromatography (MEKC) method with UV detection at 200 nm for analysis of piracetam in plasma and in cerebrospinal fluid (CSF) by direct injection without any sample pretreatment is described. The separation of piracetam from biological matrix was performed at 25 degrees C using a background electrolyte consisting of Tris buffer with sodium dodecyl sulfate (SDS) as the electrolyte solution. Several parameters affecting the separation of the drug from biological matrix were studied, including the pH and concentrations of the Tris buffer and SDS. Under optimal MEKC condition, good separation with high efficiency and short analyses time is achieved. Using imidazole as an internal standard (IS), the linear ranges of the method for the determination of piracetam in plasma and in CSF were all between 5 and 500 microg/mL; the detection limit of the drug in plasma and in CSF (signal-to-noise ratio=3; injection 0.5 psi, 5s) was 1.0 microg/mL. The applicability of the proposed method for determination of piracetam in plasma and CSF collected after intravenous administration of 3g piracetam every 6h and oral administration 1.2g every 6h in encephalopathy patients with aphasia was demonstrated.

  9. Determination of ractopamine and salbutamol in pig hair by liquid chromatography tandem mass spectrometry.

    PubMed

    Chang, Kai-Chun; Chang, Yu-Ting; Tsai, Chin-En

    2018-04-01

    A liquid chromatography tandem mass spectrometric method was developed for the determination of two β-agonists (ractopamine and salbutamol) in pig hair samples. An isotope of ractopamine-d5 or salbutamol-d6 as an internal standard was used to carry out quantitative analysis. Concentrated sodium hydroxide was used to pretreat hair samples and then purified by the solid phase extraction (SPE) procedure. The extracted solution was evaporated and reconstituted for injection in the instrument with electrospray ionization (ESI) operating in a positive multiple-reaction-monitoring (MRM) mode. Ractopamine and salbutamol separation were performed on C18 analytical column under gradient condition. The internal standard calibration curve was linear in the range of concentration from 0.5 to 100 ng mL -1  (R 2  > 0.995). Recoveries of this method estimated at three spiked concentrations of 100, 250 and 500 ng mL -1 in pig hair samples, were 79-82% for ractopamine and 77-96% for salbutamol. The corresponding inter-day and intra-day precisions expressed as relative standard deviation (RSD %) were 3.8-6.4% and 3.8-8.6%, respectively. The analytical time for one sample was 8 min. The detection limit of this method was 0.6 and 8.3 ng mL -1 for ractopamine and salbutamol, respectively. This developed method can be applied for monitoring the use of the β-agonists salbutamol and ractopamine in swine feed incurred pig hair. Copyright © 2017. Published by Elsevier B.V.

  10. Analysis of glycosaminoglycans in cerebrospinal fluid from patients with mucopolysaccharidoses by isotope-dilution ultra-performance liquid chromatography-tandem mass spectrometry.

    PubMed

    Zhang, Haoyue; Young, Sarah P; Auray-Blais, Christiane; Orchard, Paul J; Tolar, Jakub; Millington, David S

    2011-07-01

    New therapies for the treatment of mucopolysaccharidoses that target the brain, including intrathecal enzyme replacement, are being explored. Quantitative analysis of the glycosaminoglycans (GAGs) that accumulate in these disorders is required to assess the disease burden and monitor the effect of therapy in affected patients. Because current methods lack the required limit of quantification and specificity to analyze GAGs in small volumes of cerebrospinal fluid (CSF), we developed a method based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples of CSF (25 μL) were evaporated to dryness and subjected to methanolysis. The GAGs were degraded to uronic acid-N-acetylhexosamine dimers and mixed with internal standards derived from deuteriomethanolysis of GAG standards. Specific dimers derived from heparan, dermatan and chondroitin sulfates (HS, DS and CS) were separated by UPLC and analyzed by electrospray ionization MS/MS using selected reaction monitoring for each targeted GAG product and its corresponding internal standard. CSF from control pediatric subjects (n = 22) contained <0.38 mg/L HS, 0.26 mg/L DS, and 2.8 mg/L CS, whereas CSF from patients with Hurler syndrome (n = 7) contained concentrations of DS and HS that were at least 6-fold greater than the upper control limits. These concentrations were reduced by 17.5% to 82.5% after allogeneic transplantation and treatment with intrathecal and intravenous enzyme replacement therapy. The method described here has potential value in monitoring patients with mucopolysaccharidoses receiving treatment targeted to the brain.

  11. A simple, rapid and sensitive RP-HPLC-UV method for the simultaneous determination of sorafenib & paclitaxel in plasma and pharmaceutical dosage forms: Application to pharmacokinetic study.

    PubMed

    Khan, Ismail; Iqbal, Zafar; Khan, Abad; Hassan, Muhammad; Nasir, Fazle; Raza, Abida; Ahmad, Lateef; Khan, Amjad; Akhlaq Mughal, Muhammad

    2016-10-15

    A simple, economical, fast, and sensitive RP-HPLC-UV method has been developed for the simultaneous quantification of Sorafenib and paclitaxel in biological samples and formulations using piroxicam as an internal standard. The experimental conditions were optimized and method was validated according to the standard guidelines. The separation of both the analytes and internal standard was achieved on Discovery HS C18 column (250mm×4.6mm, 5μm) using Acetonitrile and TFA (0.025%) in the ratio of (65:35V/V) as the mobile phase in isocratic mode at a flow rate of 1ml/min, with a wavelength of 245nm and at a column oven temperature of 25°Cin a short run time of 12min. The limits of detection (LLOD) were 5 and 10ng/ml while the limits of quantification (LLOQ) were 10 and 15ng/ml for sorafenib and paclitaxel, respectively. Sorafenib, paclitaxel and piroxicam (IS) were extracted from biological samples by applying acetonitrile as a precipitating and extraction solvent. The method is linear in the range of 15-20,000ng/ml for paclitaxel and 10-5000ng/ml for sorafenib, respectively. The method is sensitive and reliable by considering both of its intra-day and inter-day co-efficient of variance. The method was successfully applied for the quantification of the above mentioned drugs in plasma. The developed method will be applied towards sorafenib and paclitaxel pharmacokinetics studies in animal models. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Simultaneous determination of three pesticide adjuvant residues in plant-derived agro-products using liquid chromatography-tandem mass spectrometry.

    PubMed

    Li, Hui; Jiang, Zejun; Cao, Xiaolin; Su, Hang; Shao, Hua; Jin, Fen; Abd El-Aty, A M; Wang, Jing

    2017-12-15

    Herein, an accurate and reliable isotope-labelled internal standard method was developed and validated for simultaneous determination of three polar pesticide adjuvants, namely 2-pyrrolidone, N-methyl-2-pyrrolidone, and N-ethyl-2-pyrrolidone in plant-derived agro-products. Matrices, including apple, cabbage, tomato, cucumber, rice, and wheat were extracted with a modified quick, easy, cheap, effective, rugged, and safe "QuEChERS" method and purified with a new clean-up sorbent (Z-Sep). A hydrophilic interaction liquid chromatography column (HILIC), exhibiting a lipophilic-hydrophilic character, was used to separate the three analytes over 10min using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Matrix effects in various matrices were evaluated and an isotope-labelled internal standard method was employed to compensate for ion enhancement/suppression effects. At three fortification levels (2.0, 5.0, and 20.0μg/kg), the mean recoveries ranged from 78.5 to 112.1% with relative standard deviations (RSDs)<11.0% for all tested analytes. The limits of detection (LODs) and quantification (LOQs) were 0.04-0.45 and 0.12-1.58μg/kg in various matrices, respectively. The developed experimental protocol was successfully applied to monitor different samples purchased from local markets in Beijing, China. In conclusion, the developed method exhibited both high sensitivity and satisfactory accuracy and is suitable for the simultaneous determination of the three tested pesticide adjuvant residues in agro-products of plant origin. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Second-tier test for quantification of underivatized amino acids in dry blood spot for metabolic diseases in newborn screening.

    PubMed

    Wang, Chunyan; Zhu, Hongbin; Zhang, Wenyan; Song, Fengrui; Liu, Zhiqiang; Liu, Shuying

    2013-02-01

    The quantitative analysis of amino acids (AAs) in single dry blood spot (DBS) samples is an important issue for metabolic diseases as a second-tier test in newborn screening. An analytical method for quantifying underivatized AAs in DBS was developed by using liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample preparation in this method is simple and ion-pairing agent is not used in the mobile phase that could avoid ion suppression, which happens in mass spectrometry and avoids damage to the column. Through chromatographic separation, some isomeric compounds could be identified and quantified, which cannot be solved through only appropriate multiple reactions monitoring transitions by MS/MS. The concentrations of the different AAs were determined using non-deuterated internal standard. All calibration curves showed excellent linearity within test ranges. For most of the amino acids the accuracy of extraction recovery was between 85.3 and 115 %, and the precision of relative standard deviation was <7.0 %. The 35 AAs could be identified in DBS specimens by the developed LC-MS/MS method in 17-19 min, and eventually 24 AAs in DBS were quantified. The results of the present study prove that this method as a second-tier test in newborn screening for metabolic diseases could be performed by the quantification of free AAs in DBS using the LC-MS/MS method. The assay has advantages of high sensitive, specific, and inexpensive merits because non-deuterated internal standard and acetic acid instead of ion-pairing agent in mobile phase are used in this protocol.

  14. Determination of vigabatrin in human plasma and urine by high-performance liquid chromatography with UV-Vis detection.

    PubMed

    Cetin, Sevil Müge; Atmaca, Sedef

    2004-03-26

    A simple and reliable high-performance liquid chromatographic (HPLC) method with UV-Vis detection has been developed and validated for the determination of vigabatrin (VG) in human plasma and urine. The samples were pre-column derivatizated with 1,2-naphthoquinone-4-sulphonic acid sodium salt (NQS). A good chromatographic separation was achieved on a C18 column with a mobile phase consisting of acetonitrile and 10 mM orthophosphoric acid (pH 2.5) gradient elution. Tranexamic acid was used as an internal standard (I.S.). The method was linear over the concentration range of 0.8-30.0 microg/ml for both samples. The method is precise (relative standard deviation (R.S.D.) <9.13%) and accurate (relative mean error (RME) <-8.75%); analytical recoveries were 81.07% for plasma and 83.05% for urine. The assay was applied to pharmacokinetic study in a healthy volunteer after a single oral administration of 1 g of vigabatrin.

  15. Optimized, Fast-Throughput UHPLC-DAD Based Method for Carotenoid Quantification in Spinach, Serum, Chylomicrons, and Feces.

    PubMed

    Eriksen, Jane N; Madsen, Pia L; Dragsted, Lars O; Arrigoni, Eva

    2017-02-01

    An improved UHPLC-DAD-based method was developed and validated for quantification of major carotenoids present in spinach, serum, chylomicrons, and feces. Separation was achieved with gradient elution within 12.5 min for six dietary carotenoids and the internal standard, echinenone. The proposed method provides, for all standard components, resolution > 1.1, linearity covering the target range (R > 0.99), LOQ < 0.035 mg/L, and intraday and interday RSDs < 2 and 10%, respectively. Suitability of the method was tested on biological matrices. Method precision (RSD%) for carotenoid quantification in serum, chylomicrons, and feces was below 10% for intra- and interday analysis, except for lycopene. Method accuracy was consistent with mean recoveries ranging from 78.8 to 96.9% and from 57.2 to 96.9% for all carotenoids, except for lycopene, in serum and feces, respectively. Additionally, an interlaboratory validation study on spinach at two institutions showed no significant differences in lutein or β-carotene content, when evaluated on four occasions.

  16. RP-HPLC method with electrochemical detection for the determination of metoclopramide in serum and its use in pharmacokinetic studies.

    PubMed

    Lamparczyk, H; Chmielewska, A; Konieczna, L; Plenis, A; Zarzycki, P K

    2001-12-01

    A rapid and sensitive reversed-phase high performance liquid chromatographic method has been developed for the determination of metoclopramide in serum. The assay was performed after single extraction with ethyl ether using methyl parahydroxybenzoate as internal standard. Chromatographic separations were performed on C(18) stationary phase with a mobile phase composed of methanol-phosphate buffer pH 3 (30:70 v/v). Analytes were detected electrochemically. The quantification limit for metoclopramide in serum was 2 ng mL(-1). Linearity of the method was confirmed in the range of 5-120 ng mL(-1) (correlation coefficient 0.9998). Within-day relative standard deviations (RSDs) ranged from 0.3 to 5.5% and between-day RSDs from 0.8 to 6.0%. The analytical method was successfully applied for the determination of pharmacokinetic parameters after ingestion of 10 mg dose of metoclopramide. Studies were performed on 18 healthy volunteers of both sexes. Copyright 2001 John Wiley & Sons, Ltd.

  17. Determination of ibuprofen and flurbiprofen in pharmaceuticals by capillary zone electrophoresis.

    PubMed

    Hamoudová, Rafifa; Pospísilová, Marie

    2006-06-16

    Capillary zone electrophoresis with spectrophotometric detection was used for the determination of ibuprofen (IB) and flurbiprofen (FL) in pharmaceuticals. The separation was carried out in a fused silica capillary (60 cm x 100 microm i.d. effective length 45 cm) at 30 kV with UV detection at 232 nm. The optimized background electrolyte was 20mM N-(2-acetamido)-2-aminoethanesulfonic acid (ACES) with 20mM imidazole and 10mM alpha-cyclodextrin of pH 7.3. 2-Naphthoxyacetic acid was used as internal standard. A single analysis took less than 5 min. Rectilinear calibration ranges were 2-500 mg l(-1) for IB and 1-60 mg l(-1) for FL. The relative standard deviations (R.S.D.) values (n=6) were 1.53% for IB and 1.29% for FL (for 200 mg l(-1) IB and 10 mg l(-1) FL). This validated method has been successfully applied for the routine analysis of 10 commercially available pharmaceutical preparations (syrup, tablets, cream and gel).

  18. Quantification of abscisic acid in grapevine leaf (Vitis vinifera) by isotope-dilution liquid chromatography-mass spectrometry.

    PubMed

    Vilaró, Francisca; Canela-Xandri, Anna; Canela, Ramon

    2006-09-01

    A specific, sensitive, precise, and accurate method for the determination of abscisic acid (ABA) in grapevine leaf tissues is described. The method employs high-performance liquid chromatography and electrospray ionization-mass spectrometry (LC-ESI-MS) in selected ion monitoring mode (SIM) to analyze ABA using a stable isotope-labeled ABA as an internal standard. Absolute recoveries ranged from 72% to 79% using methanol/water pH 5.5 (50:50 v/v) as an extraction solvent. The best efficiency was obtained when the chromatographic separation was carried out by using a porous graphitic carbon (PGC) column. The statistical evaluation of the method was satisfactory in the work range. A relative standard deviation (RDS) of < 5.5% and < 6.0% was obtained for intra-batch and inter-batch comparisons, respectively. As for accuracy, the relative error (%Er) was between -2.7 and 4.3%, and the relative recovery ranged from 95% to 107%.

  19. J functions for the process ud→WA

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

    Bardin, D. Yu., E-mail: bardin@nu.jinr.ru; Kalinovskaya, L. V., E-mail: kalinov@mail.cern.ch; Uglov, E. D., E-mail: e.uglov@gmail.com

    In this paper we present a description of the universal approach for analytic calculations for a certain class of J functions for six topologies of the boxes for the process ud → WA. These functions J arise at the reduction of the infrared divergent box diagrams. The standard Passarino–Veltman reduction of the four-point box diagram with an internal photon line connecting two external lines on the mass shell leads to infrared-divergent and mass-singular D{sub 0} functions. In the system SANC a systematic procedure is adopted to separate both types of singularities into the simplest objects, namely C{sub 0} functions. Themore » functions J, in turn, are represented as certain linear combinations of the standard D{sub 0} and C{sub 0} functions. The subtracted J functions are free of both types of singularities and are expressed as explicit and compact linear combinations of dilogarithm functions. We present extensive comparisons of numerical results of SANC with those obtained with the aid of the LoopTools package.« less

  20. Liquid chromatography tandem mass spectrometry assay to determine the pharmacokinetics of aildenafil in human plasma.

    PubMed

    Wang, Jiang; Jiang, Yao; Wang, Yingwu; Zhao, Xia; Cui, Yimin; Gu, Jingkai

    2007-05-09

    A simple, sensitive and specific liquid chromatography/tandem mass spectrometry method for the quantitation of aildenafil, a new phosphodiesterase V inhibitor, in human plasma is presented. The analyte and internal standard, sildenafil, were extracted by a one-step liquid-liquid extraction in alkaline conditions and separated on a C(18) column using ammonia:10mM ammonium acetate buffer:methanol (0.1:15:85, v/v/v) as the mobile phase. The detection by an API 4000 triple quadrupole mass spectrometer in multiple-reaction monitoring mode was completed within 2.5 min. The calibration curve exhibited a linear dynamic range of 0.05-100 ng/ml with a 10 pg/ml limit of detection. The intra- and inter-day precisions measured as relative standard deviation were within 8.04% and 5.72%, respectively. This method has been used in a pharmacokinetic study of aildenafil in healthy male volunteers each given an oral administration of one of the three dosages.

  1. Halogenated Peptides as Internal Standards (H-PINS)

    PubMed Central

    Mirzaei, Hamid; Brusniak, Mi-Youn; Mueller, Lukas N.; Letarte, Simon; Watts, Julian D.; Aebersold, Ruedi

    2009-01-01

    As the application for quantitative proteomics in the life sciences has grown in recent years, so has the need for more robust and generally applicable methods for quality control and calibration. The reliability of quantitative proteomics is tightly linked to the reproducibility and stability of the analytical platforms, which are typically multicomponent (e.g. sample preparation, multistep separations, and mass spectrometry) with individual components contributing unequally to the overall system reproducibility. Variations in quantitative accuracy are thus inevitable, and quality control and calibration become essential for the assessment of the quality of the analyses themselves. Toward this end, the use of internal standards cannot only assist in the detection and removal of outlier data acquired by an irreproducible system (quality control) but can also be used for detection of changes in instruments for their subsequent performance and calibration. Here we introduce a set of halogenated peptides as internal standards. The peptides are custom designed to have properties suitable for various quality control assessments, data calibration, and normalization processes. The unique isotope distribution of halogenated peptides makes their mass spectral detection easy and unambiguous when spiked into complex peptide mixtures. In addition, they were designed to elute sequentially over an entire aqueous to organic LC gradient and to have m/z values within the commonly scanned mass range (300–1800 Da). In a series of experiments in which these peptides were spiked into an enriched N-glycosite peptide fraction (i.e. from formerly N-glycosylated intact proteins in their deglycosylated form) isolated from human plasma, we show the utility and performance of these halogenated peptides for sample preparation and LC injection quality control as well as for retention time and mass calibration. Further use of the peptides for signal intensity normalization and retention time synchronization for selected reaction monitoring experiments is also demonstrated. PMID:19411281

  2. 26 CFR 25.2701-7 - Separate interests.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 26 Internal Revenue 14 2011-04-01 2010-04-01 true Separate interests. 25.2701-7 Section 25.2701-7... GIFT TAX; GIFTS MADE AFTER DECEMBER 31, 1954 Special Valuation Rules § 25.2701-7 Separate interests..., prescribe rules under which an applicable retained interest is treated as two or more separate interests for...

  3. 26 CFR 25.2701-7 - Separate interests.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 26 Internal Revenue 14 2010-04-01 2010-04-01 false Separate interests. 25.2701-7 Section 25.2701-7... GIFT TAX; GIFTS MADE AFTER DECEMBER 31, 1954 Special Valuation Rules § 25.2701-7 Separate interests..., prescribe rules under which an applicable retained interest is treated as two or more separate interests for...

  4. Impact of the reduced vertical separation minimum on the domestic United States

    DOT National Transportation Integrated Search

    2009-01-31

    Aviation regulatory bodies have enacted the reduced vertical separation minimum standard over most of the globe. The reduced vertical separation minimum is a technique that reduces the minimum vertical separation distance between aircraft from 2000 t...

  5. Radiation safety standards and their application: international policies and current issues.

    PubMed

    González, Abel J

    2004-09-01

    This paper briefly describes the current policies of the United Nations Scientific Committee on the Effects of Atomic Radiation and the International Commission on Radiological Protection and how these policies are converted into international radiation safety standards by the International Atomic Energy Agency, which is the only global organization-within the United Nations family of international agencies-with a statutory mandate not only to establish such standards but also to provide for their application. It also summarizes the current status of the established corpus of such international standards, and of it foreseeable evolution, as well as of legally binding undertakings by countries around the world that are linked to these standards. Moreover, this paper also reviews some major current global issues related to the application of international standards, including the following: strengthening of national infrastructures for radiation safety, including technical cooperation programs for assisting developing countries; occupational radiation safety challenges, including the protection of pregnant workers and their unborn children, dealing with working environments with high natural radiation levels, and occupational attributability of health effects (probability of occupational causation); restricting discharges of radioactive substances into the environment: reviewing current international policies vis-a-vis the growing concern on the radiation protection of the "environment;" radiological protection of patients undergoing radiodiagnostic and radiotherapeutic procedures: the current International Action Plan; safety and security of radiation sources: post-11 September developments; preparedness and response to radiation emergencies: enhancing the international network; safe transport of radioactive materials: new apprehensions; safety of radioactive waste management: concerns and connections with radiation protection; and radioactive residues remaining after the termination of activities: radiation protection response to the forthcoming wave of decommissioning of installations with radioactive materials. The ultimate aim of this paper is to encourage information exchange, cooperation, and collaboration within the radiation protection professional community. In particular, the paper tries to facilitate consolidation of the growing international regime on radiation safety, including the expansion of legally binding undertakings by countries, the strengthening of the current corpus of international radiation safety standards, and the development of international provisions for ensuring the proper worldwide application of these standards, such as a system of international appraisals by peer review.

  6. 46 CFR 133.03 - Relationship to international standards.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 46 Shipping 4 2011-10-01 2011-10-01 false Relationship to international standards. 133.03 Section 133.03 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) OFFSHORE SUPPLY VESSELS LIFESAVING SYSTEMS General § 133.03 Relationship to international standards. This subpart and subpart B of...

  7. 77 FR 60625 - Minimum Internal Control Standards for Class II Gaming

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-10-04

    ...-37 Minimum Internal Control Standards for Class II Gaming AGENCY: National Indian Gaming Commission... Internal Control Standards that were published on September 21, 2012. DATES: The effective date [email protected] . FOR FURTHER INFORMATION CONTACT: Jennifer Ward, Attorney, NIGC Office of General Counsel, at...

  8. 46 CFR 133.03 - Relationship to international standards.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 46 Shipping 4 2014-10-01 2014-10-01 false Relationship to international standards. 133.03 Section 133.03 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) OFFSHORE SUPPLY VESSELS LIFESAVING SYSTEMS General § 133.03 Relationship to international standards. This subpart and subpart B of...

  9. 46 CFR 133.03 - Relationship to international standards.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 46 Shipping 4 2012-10-01 2012-10-01 false Relationship to international standards. 133.03 Section 133.03 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) OFFSHORE SUPPLY VESSELS LIFESAVING SYSTEMS General § 133.03 Relationship to international standards. This subpart and subpart B of...

  10. 46 CFR 133.03 - Relationship to international standards.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 46 Shipping 4 2010-10-01 2010-10-01 false Relationship to international standards. 133.03 Section 133.03 Shipping COAST GUARD, DEPARTMENT OF HOMELAND SECURITY (CONTINUED) OFFSHORE SUPPLY VESSELS LIFESAVING SYSTEMS General § 133.03 Relationship to international standards. This subpart and subpart B of...

  11. 25 CFR 543.14 - What are the minimum internal control standards for patron deposit accounts and cashless systems?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for patron deposit accounts and cashless systems? 543.14 Section 543.14 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.14 What are the minimum internal control...

  12. 25 CFR 542.4 - How do these regulations affect minimum internal control standards established in a Tribal-State...

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 25 Indians 2 2010-04-01 2010-04-01 false How do these regulations affect minimum internal control standards established in a Tribal-State compact? 542.4 Section 542.4 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.4 How do these regulations affect minimum internal...

  13. 25 CFR 542.4 - How do these regulations affect minimum internal control standards established in a Tribal-State...

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 25 Indians 2 2011-04-01 2011-04-01 false How do these regulations affect minimum internal control standards established in a Tribal-State compact? 542.4 Section 542.4 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.4 How do these regulations affect minimum internal...

  14. 25 CFR 543.12 - What are the minimum internal control standards for gaming promotions and player tracking systems?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for gaming promotions and player tracking systems? 543.12 Section 543.12 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.12 What are the minimum internal contro...

  15. 25 CFR 542.4 - How do these regulations affect minimum internal control standards established in a Tribal-State...

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false How do these regulations affect minimum internal control standards established in a Tribal-State compact? 542.4 Section 542.4 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.4 How do these regulations affect minimum internal...

  16. 25 CFR 542.4 - How do these regulations affect minimum internal control standards established in a Tribal-State...

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... 25 Indians 2 2012-04-01 2012-04-01 false How do these regulations affect minimum internal control standards established in a Tribal-State compact? 542.4 Section 542.4 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.4 How do these regulations affect minimum internal...

  17. 25 CFR 543.14 - What are the minimum internal control standards for patron deposit accounts and cashless systems?

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... 25 Indians 2 2013-04-01 2013-04-01 false What are the minimum internal control standards for patron deposit accounts and cashless systems? 543.14 Section 543.14 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.14 What are the minimum internal control...

  18. 25 CFR 542.4 - How do these regulations affect minimum internal control standards established in a Tribal-State...

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false How do these regulations affect minimum internal control standards established in a Tribal-State compact? 542.4 Section 542.4 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS § 542.4 How do these regulations affect minimum internal...

  19. 25 CFR 543.12 - What are the minimum internal control standards for gaming promotions and player tracking systems?

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... 25 Indians 2 2014-04-01 2014-04-01 false What are the minimum internal control standards for gaming promotions and player tracking systems? 543.12 Section 543.12 Indians NATIONAL INDIAN GAMING COMMISSION, DEPARTMENT OF THE INTERIOR HUMAN SERVICES MINIMUM INTERNAL CONTROL STANDARDS FOR CLASS II GAMING § 543.12 What are the minimum internal contro...

  20. 47 CFR 76.612 - Cable television frequency separation standards.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... frequency separation standards. All cable television systems which operate in the frequency bands 108-137... kHz bandwidth in any 160 microsecond period must operate at frequencies offset from certain frequencies which may be used by aeronautical radio services operated by Commission licensees or by the United...

  1. Status of international optical disk standards

    NASA Astrophysics Data System (ADS)

    Chen, Di; Neumann, John

    1999-11-01

    Optical technology for data storage offers media removability with unsurpassed reliability. As the media are removable, data interchange between the media and drives from different sources is a major concern. The optical recording community realized, at the inception of this new storage technology development, that international standards for all optical recording disk/cartridge must be established to insure the healthy growth of this industry and for the benefit of the users. Many standards organizations took up the challenge and numerous international standards were established which are now being used world-wide. This paper provides a brief summary of the current status of the international optical disk standards.

  2. Measurement of Henry's Law Constants Using Internal Standards: A Quantitative GC Experiment for the Instrumental Analysis or Environmental Chemistry Laboratory

    ERIC Educational Resources Information Center

    Ji, Chang; Boisvert, Susanne M.; Arida, Ann-Marie C.; Day, Shannon E.

    2008-01-01

    An internal standard method applicable to undergraduate instrumental analysis or environmental chemistry laboratory has been designed and tested to determine the Henry's law constants for a series of alkyl nitriles. In this method, a mixture of the analytes and an internal standard is prepared and used to make a standard solution (organic solvent)…

  3. Test-retest reliability of cardinal plane isokinetic hip torque and EMG.

    PubMed

    Claiborne, Tina L; Timmons, Mark K; Pincivero, Danny M

    2009-10-01

    The objective of the present study was to establish test-retest reliability of isokinetic hip torque and prime mover electromyogram (EMG) through the three cardinal planes of motion. Thirteen healthy young adults participated in two experimental sessions, separated by approximately one week. During each session, isokinetic hip torque was evaluated on the Biodex Isokinetic Dynamometer at a velocity of 60 deg/s. Subjects performed three maximal-effort concentric and eccentric contractions, separately, for right and left hip abduction/adduction, flexion/extension, and internal/external rotation. Surface EMGs were sampled from the gluteus maximus, gluteus medius, adductor, medial and lateral hamstring, and rectus femoris muscles during all contractions. Intraclass correlation coefficients (ICC - 2,1) and standard errors of measurement (SEM) were calculated for peak torque for each movement direction and contraction mode, while ICCs were only computed for the EMG data. Motions that demonstrated high torque reliability included concentric hip abduction (right and left), flexion (right and left), extension (right) and internal rotation (right and left), and eccentric hip abduction (left), adduction (left), flexion (right), and extension (right and left) (ICC range=0.81-0.91). Motions with moderate torque reliability included concentric hip adduction (right), extension (left), internal rotation (left), and external rotation (right), and eccentric hip abduction and adduction (right), flexion (left), internal rotation (right and left), and external rotation (right and left) (ICC range=0.49-0.79). The majority of the EMG sampled muscles (n=12 and n=11 for concentric and eccentric contractions, respectively) demonstrated high reliability (ICC=0.81-0.95). Instances of low, or unacceptable, EMG reliability values occurred for the medial hamstring muscle of the left leg (both contraction modes) and the adductor muscle of the right leg during eccentric internal rotation. The major finding revealed high and moderate levels of between-day reliability of isokinetic hip peak torque and prime mover EMG. It is recommended that the day-to-day variability estimates concomitant with acceptable levels of reliability be considered when attempting to objectify intervention effects on hip muscle performance.

  4. 40 CFR 312.11 - References.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... the requirements set forth in §§ 312.23 through 312.31: (a) The procedures of ASTM International... Site Assessment Process.” (b) The procedures of ASTM International Standard E2247-08 entitled “Standard... or Rural Property.” This standard is available from ASTM International at http://www.astm.org, 1-610...

  5. 78 FR 14457 - National Emission Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-03-06

    ... ENVIRONMENTAL PROTECTION AGENCY 40 CFR Parts 60 and 63 [EPA-HQ-OAR-2008-0708, FRL-9756-4] RIN 2060-AQ58 National Emission Standards for Hazardous Air Pollutants for Reciprocating Internal Combustion Engines; New Source Performance Standards for Stationary Internal Combustion Engines Correction In rule...

  6. Internal Standards: A Source of Analytical Bias For Volatile Organic Analyte Determinations

    EPA Science Inventory

    The use of internal standards in the determination of volatile organic compounds as described in SW-846 Method 8260C introduces a potential for bias in results once the internal standards (ISTDs) are added to a sample for analysis. The bias is relative to the dissimilarity betw...

  7. The influence of international standards on optomechanical design

    NASA Astrophysics Data System (ADS)

    Parks, Robert E.

    1992-12-01

    In the last 10 to 15 years, a considerable body of international standards literature has been published on both mechanical and optical design. We discuss the influence of these internationally developed standards on the design and fabrication of optical systems. We conclude that while there are large benefits to be gained from using these international standards, there will have to be a substantial educational effort at all levels from project scientist to worker on the shop floor to take advantage of the benefits. Many sources to help in this education process are outlined.

  8. INTERNATIONAL REPORTS: New International Standards for Quantities and Units

    NASA Astrophysics Data System (ADS)

    Thor, A. J.

    1994-01-01

    Each coherent system of units is based on a system of quantities in such a way that the equations between the numerical values expressed in coherent units have exactly the same form, including numerical factors, as the corresponding equations between the quantities. The highest international body responsible for the International System of Units (SI) is the Conférence Générale des Poids et Mesures (CGPM). However, the CGPM is not concerned with quantities or systems of quantities. That question lies within the scope of Technical Committee number twelve of the International Organization for Standardization (ISO/TC 12). Quantities, units, symbols, conversion factors. To fulfil its responsibility, ISO/TC 12 has prepared the International Standard ISO 31, Quantities and Units, which consists of fourteen parts. The new editions of the different parts of the International Standard are briefly presented here.

  9. Broadband arrayed waveguide grating multiplexers on indium phosphide

    NASA Astrophysics Data System (ADS)

    Rausch, Kameron

    2005-11-01

    Coarse Wavelength Division Multiplexing (CWDM) is becoming a popular way to increase the optical throughput of fibers for short to medium haul networks at a reduced cost. The International Telecommunications Union (ITU) has defined the CWDM network to consist of eighteen channels with channel spacings of 20 nm starting at 1270 nm and ending at 1610 nm. Four and eight channel AWGs suitable for CWDM were fabricated using a versatile S-shape design novel to InP. The standard horseshoe layout will not work on semiconductor for AWGs with a free spectral range (FSR) larger than 30 nm. The AWG design provides operation insensitive to thermal and polarization fluctuations; which is key for low cost operation and packaging. It will be shown that, refractive index changes over the large operating wavelength band produced negligible effects in the transmission spectrum. Standard AWG design assumes refractive index is a constant over the operating wavelength band. As a result, the output waveguide separations are held constant on the second star coupler. As the channel number increases, secondary focal dispersion caused from a changing refractive index can have detrimental effects on performance. A new design method will be introduced which includes refractive index dispersion by allowing the output waveguide separations to vary. The new design is consistent with standard design but is applicable in materials with a linear index dispersion over an arbitrarily large wavelength band. Lastly, a method for increasing the transmission using multimode waveguides is discussed. Traditionally, single mode waveguides are required in order to prevent higher order waveguide modes creating ghost images in the output spectrum. Using bend loss and waveguide junction offsets, higher order modes can be filtered from the output, thereby eliminating ghost images and at the same time, increase transmission.

  10. Resonance scattering of a dielectric sphere illuminated by electromagnetic Bessel non-diffracting (vortex) beams with arbitrary incidence and selective polarizations

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

    Mitri, F.G., E-mail: F.G.Mitri@ieee.org; Li, R.X., E-mail: rxli@mail.xidian.edu.cn; Collaborative Innovation Center of Information Sensing and Understanding, Xidian University, Xi’an 710071

    A complete description of vector Bessel (vortex) beams in the context of the generalized Lorenz–Mie theory (GLMT) for the electromagnetic (EM) resonance scattering by a dielectric sphere is presented, using the method of separation of variables and the subtraction of a non-resonant background (corresponding to a perfectly conducting sphere of the same size) from the standard Mie scattering coefficients. Unlike the conventional results of standard optical radiation, the resonance scattering of a dielectric sphere in air in the field of EM Bessel beams is examined and demonstrated with particular emphasis on the EM field’s polarization and beam order (or topologicalmore » charge). Linear, circular, radial, azimuthal polarizations as well as unpolarized Bessel vortex beams are considered. The conditions required for the resonance scattering are analyzed, stemming from the vectorial description of the EM field using the angular spectrum decomposition, the derivation of the beam-shape coefficients (BSCs) using the integral localized approximation (ILA) and Neumann–Graf’s addition theorem, and the determination of the scattering coefficients of the sphere using Debye series. In contrast with the standard scattering theory, the resonance method presented here allows the quantitative description of the scattering using Debye series by separating diffraction effects from the external and internal reflections from the sphere. Furthermore, the analysis is extended to include rainbow formation in Bessel beams and the derivation of a generalized formula for the deviation angle of high-order rainbows. Potential applications for this analysis include Bessel beam-based laser imaging spectroscopy, atom cooling and quantum optics, electromagnetic instrumentation and profilometry, optical tweezers and tractor beams, to name a few emerging areas of research.« less

  11. Optimization and validation of the reversed-phase high-performance liquid chromatography with fluorescence detection method for the separation of tocopherol and tocotrienol isomers in cereals, employing a novel sorbent material.

    PubMed

    Irakli, Maria N; Samanidou, Victoria F; Papadoyannis, Ioannis N

    2012-03-07

    The separation and determination of tocopherols (Ts) and tocotrienols (T3s) by reversed-phase high-performance liquid chromatography with fluorescence detection has been developed and validated after optimization of various chromatographic conditions and other experimental parameters. Analytes were separated on a PerfectSil Target ODS-3 (250 × 4.6 mm, 3 μm) column filled with a novel sorbent material of ultrapure silica gel. The separation of Ts and T3s was optimized in terms of mobile-phase composition and column temperature on the basis of the best compromise among efficiency, resolution, and analysis time. Using a gradient elution of mobile phase composed of isopropanol/water and 7 °C column temperature, a satisfactory resolution was achieved within 62 min. For the quantitative determination, α-T acetate (50 μg/mL) was used as the internal standard. Detection limits ranged from 0.27 μg/mL (γ-T) to 0.76 μg/mL (γ-T3). The validation of the method was examined performing intraday (n = 5) and interday (n = 3) assays and was found to be satisfactory, with high accuracy and precision results. Solid-phase extraction provided high relative extraction recoveries from cereal samples: 87.0% for γ-T3 and 115.5% for δ-T. The method was successfully applied to cereals, such as durum wheat, bread wheat, rice, barley, oat, rye, and corn.

  12. Enhanced capabilities of separation in Sequential Injection Chromatography--fused-core particle column and its comparison with narrow-bore monolithic column.

    PubMed

    Chocholouš, Petr; Kosařová, Lucie; Satínský, Dalibor; Sklenářová, Hana; Solich, Petr

    2011-08-15

    In the Sequential Injection Chromatography (SIC) only monolithic columns for chromatographic separations have been used so far. This article presents the first use of fused-core particle packed column in an attempt to extend of the chromatographic capabilities of the SIC system. A new fused-core particle column (2.7 μm) Ascentis(®) Express C18 (Supelco™ Analytical) 30 mm × 4.6 mm brings high separation efficiency within flow rates and pressures comparable to monolithic column Chromolith(®) Performance RP-18e 100-3 (Merck(®)) 100 mm × 3 mm. Both columns matches the conditions of the commercially produced SIC system - SIChrom™ (8-port high-pressure selection valve and medium-pressure Sapphire™ syringe pump with 4 mL reservoir - maximal work pressure 1000 PSI) (FIAlab(®), USA). The system was tested by the separation of four estrogens with similar structure and an internal standard - ethylparaben. The mobile phase composed of acetonitrile/water (40/60 (v/v)) was pumped isocratic at flow rate 0.48 mL min(-1). Spectrophotometric detection was performed at wavelength of 225 nm and injected volume of sample solutions was 10 μL. The chromatographic characteristics of both columns were compared. Obtained results and conclusions have shown that both fused-core particle column and longer narrow shaped monolithic column bring benefits into the SIC method. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. CTEPP STANDARD OPERATING PROCEDURE FOR PREPARATION OF SURROGATE RECOVERY STANDARD AND INTERNAL STANDARD SOLUTIONS FOR POLAR TARGET ANALYTES (SOP-5.26)

    EPA Science Inventory

    This SOP describes the method used for preparing surrogate recovery standard and internal standard solutions for the analysis of polar target analytes. It also describes the method for preparing calibration standard solutions for polar analytes used for gas chromatography/mass sp...

  14. 26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's... residual shared employee as defined in § 1.414(r)-11(b)(2) and (4)) is assigned to a single qualified...

  15. 26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's... residual shared employee as defined in § 1.414(r)-11(b)(2) and (4)) is assigned to a single qualified...

  16. 26 CFR 1.414(r)-4 - Qualified separate line of business-fifty-employee and notice requirements.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ...-employee and notice requirements. 1.414(r)-4 Section 1.414(r)-4 Internal Revenue INTERNAL REVENUE SERVICE... Bonus Plans, Etc. § 1.414(r)-4 Qualified separate line of business—fifty-employee and notice... business (as determined under § 1.414(r)-3) satisfies the 50-employee and notice requirements of § 1.414(r...

  17. 26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's... residual shared employee as defined in § 1.414(r)-11(b)(2) and (4)) is assigned to a single qualified...

  18. 26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE..., Profit-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's... residual shared employee as defined in § 1.414(r)-11(b)(2) and (4)) is assigned to a single qualified...

  19. 26 CFR 1.414(r)-7 - Determination of the employees of an employer's qualified separate lines of business.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... qualified separate lines of business. 1.414(r)-7 Section 1.414(r)-7 Internal Revenue INTERNAL REVENUE...-Sharing, Stock Bonus Plans, Etc. § 1.414(r)-7 Determination of the employees of an employer's qualified... residual shared employee as defined in § 1.414(r)-11(b)(2) and (4)) is assigned to a single qualified...

  20. 7 CFR 51.1584 - Internal discoloration.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... STANDARDS) United States Consumer Standards for Potatoes Definitions § 51.1584 Internal discoloration..., stem-end browning, internal brown spot, or other similar types of discoloration not visible externally. ...

  1. 7 CFR 51.1584 - Internal discoloration.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... STANDARDS) United States Consumer Standards for Potatoes Definitions § 51.1584 Internal discoloration..., stem-end browning, internal brown spot, or other similar types of discoloration not visible externally. ...

  2. Operations and Plans: International Military Rationalization, Standardization, and Interoperability

    DTIC Science & Technology

    1989-02-15

    Army Regulation 34–1 Operations and Plans International Military Rationalization , Standardization, and Interoperability Headquarters Department of...YYYY) 15-02-1997 2. REPORT TYPE 3. DATES COVERED (FROM - TO) xx-xx-1997 to xx-xx-1997 4. TITLE AND SUBTITLE International Military Rationalization ...DSN 427-9007 Standard Form 298 (Rev. 8-98) Prescribed by ANSI Std Z39.18 SUMMARY of CHANGE AR 34–1 International Military Rationalization

  3. 46 CFR 80.25 - Notification of safety standards.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... standards, except the 1966 fire safety standards. (ii) This vessel complies with international safety standards developed prior to 1960. There is (or, is not) an automatic sprinkler system fitted in the... international safety standard. There is (or, is not) an automatic sprinkler system fitted in the passenger...

  4. 46 CFR 80.25 - Notification of safety standards.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... standards, except the 1966 fire safety standards. (ii) This vessel complies with international safety standards developed prior to 1960. There is (or, is not) an automatic sprinkler system fitted in the... international safety standard. There is (or, is not) an automatic sprinkler system fitted in the passenger...

  5. 46 CFR 80.25 - Notification of safety standards.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... standards, except the 1966 fire safety standards. (ii) This vessel complies with international safety standards developed prior to 1960. There is (or, is not) an automatic sprinkler system fitted in the... international safety standard. There is (or, is not) an automatic sprinkler system fitted in the passenger...

  6. 46 CFR 80.25 - Notification of safety standards.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... standards, except the 1966 fire safety standards. (ii) This vessel complies with international safety standards developed prior to 1960. There is (or, is not) an automatic sprinkler system fitted in the... international safety standard. There is (or, is not) an automatic sprinkler system fitted in the passenger...

  7. The International Standard for Oxytetracycline

    PubMed Central

    Humphrey, J. H.; Lightbown, J. W.; Mussett, M. V.; Perry, W. L. M.

    1955-01-01

    The first attempt to set up an international standard for oxytetracycline, using oxytetracycline hydrochloride, failed because of difficulties in obtaining a preparation whose moisture content was uniform after distribution into ampoules. A preparation of dihydrate of oxytetracycline base was obtained instead, and was compared in an international collaborative assay with a sample of oxytetracycline hydrochloride, which was the current working standard of Chas. Pfizer & Co., Inc., USA. The results of the collaborative assay showed that the potency of the dihydrate was uniform, and that it was a suitable preparation for use as the International Standard. Evidence was obtained, however, that the reference preparation at the time of examination was less potent than had been originally supposed, and that it was hydrated. The potency of the proposed international standard was recalculated after allowance for water in the reference preparation, and the resulting biological potency agreed well with that to be expected on the basis of the physicochemical properties of the preparation. It was agreed, therefore, that the recalculated values should be used, and the preparation of oxytetracycline base dihydrate used in the collaborative assay is established as the International Standard for Oxytetracycline with a potency of 900 International Units per mg. PMID:13284563

  8. No Longer Have to Choose

    NASA Astrophysics Data System (ADS)

    Brown, H.; Ritchey, N. A.

    2017-12-01

    NOAA National Centers for Environmental Information (NCEI) once was three separate data centers (NGDC, NODC, and NCDC). In 2015 the three centers merged into NCEI. NCEI has refined the art of long term preservation and stewardship practices throughout the life-cycle of various types of data. NCEI can help you navigate and make the complicated world of preserving your data user-friendly. Using tools at NCEI, data providers can request data to be archived, submit data for archival and create complete International Organization for Standardization (ISO) metadata records with ease. To ensure traceability, Digital Object Identifiers (DOIs) are minted for published data sets. The services offered at NCEI follow standards and NOAA directives such as the Open Archival Information System (OAIS) - Reference Model (ISO 14721) to ensure consistent long-term preservation for the Nation's resource of global environmental data for a broad spectrum of users. The implementation of these standards supports the data to be accessible, independently understandable and reproducible in an easy to understand format for all types of users. Insights from combined knowledge of 100+years of various domain and data management and preservation and the tools supporting these functions will be shared.

  9. A routine high-precision method for Lu-Hf isotope geochemistry and chronology

    USGS Publications Warehouse

    Patchett, P.J.; Tatsumoto, M.

    1981-01-01

    A method for chemical separation of Lu and Hf from rock, meteorite and mineral samples is described, together with a much improved mass spectrometric running technique for Hf. This allows (i) geo- and cosmochronology using the176Lu???176Hf+??- decay scheme, and (ii) geochemical studies of planetary processes in the earth and moon. Chemical yields for the three-stage ion-exchange column procedure average 90% for Hf. Chemical blanks are <0.2 ng for Lu and Hf. From 1 ??g of Hf, a total ion current of 0.5??10-11 Ampere can be maintained for 3-5 h, yielding 0.01-0.03% precision on the ratio176Hf/177Hf. Normalisation to179Hf/177Hf=0.7325 is used. Extensive results for the Johnson Matthey Hf standard JMC 475 are presented, and this sample is urged as an international mass spectrometric standard; suitable aliquots, prepared from a single batch of JMC 475, are available from Denver. Lu-Hf analyses of the standard rocks BCR-1 and JB-1 are given. The potential of the Lu-Hf method in isotope geochemistry is assessed. ?? 1980 Springer-Verlag.

  10. 40 CFR 60.4206 - How long must I meet the emission standards if I am an owner or operator of a stationary CI...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... standards if I am an owner or operator of a stationary CI internal combustion engine? 60.4206 Section 60... Ignition Internal Combustion Engines Emission Standards for Owners and Operators § 60.4206 How long must I meet the emission standards if I am an owner or operator of a stationary CI internal combustion engine...

  11. 40 CFR 60.4206 - How long must I meet the emission standards if I am an owner or operator of a stationary CI...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... standards if I am an owner or operator of a stationary CI internal combustion engine? 60.4206 Section 60... Ignition Internal Combustion Engines Emission Standards for Owners and Operators § 60.4206 How long must I meet the emission standards if I am an owner or operator of a stationary CI internal combustion engine...

  12. 40 CFR 60.4234 - How long must I meet the emission standards if I am an owner or operator of a stationary SI...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... standards if I am an owner or operator of a stationary SI internal combustion engine? 60.4234 Section 60... Internal Combustion Engines Emission Standards for Owners and Operators § 60.4234 How long must I meet the emission standards if I am an owner or operator of a stationary SI internal combustion engine? Owners and...

  13. 40 CFR 60.4234 - How long must I meet the emission standards if I am an owner or operator of a stationary SI...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... standards if I am an owner or operator of a stationary SI internal combustion engine? 60.4234 Section 60... Internal Combustion Engines Emission Standards for Owners and Operators § 60.4234 How long must I meet the emission standards if I am an owner or operator of a stationary SI internal combustion engine? Owners and...

  14. 40 CFR 60.4206 - How long must I meet the emission standards if I am an owner or operator of a stationary CI...

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... standards if I am an owner or operator of a stationary CI internal combustion engine? 60.4206 Section 60... Ignition Internal Combustion Engines Emission Standards for Owners and Operators § 60.4206 How long must I meet the emission standards if I am an owner or operator of a stationary CI internal combustion engine...

  15. 40 CFR 60.4234 - How long must I meet the emission standards if I am an owner or operator of a stationary SI...

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... standards if I am an owner or operator of a stationary SI internal combustion engine? 60.4234 Section 60... Internal Combustion Engines Emission Standards for Owners and Operators § 60.4234 How long must I meet the emission standards if I am an owner or operator of a stationary SI internal combustion engine? Owners and...

  16. 40 CFR 60.4234 - How long must I meet the emission standards if I am an owner or operator of a stationary SI...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... standards if I am an owner or operator of a stationary SI internal combustion engine? 60.4234 Section 60... Internal Combustion Engines Emission Standards for Owners and Operators § 60.4234 How long must I meet the emission standards if I am an owner or operator of a stationary SI internal combustion engine? Owners and...

  17. 40 CFR 60.4234 - How long must I meet the emission standards if I am an owner or operator of a stationary SI...

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... standards if I am an owner or operator of a stationary SI internal combustion engine? 60.4234 Section 60... Internal Combustion Engines Emission Standards for Owners and Operators § 60.4234 How long must I meet the emission standards if I am an owner or operator of a stationary SI internal combustion engine? Owners and...

  18. Determination of aesculin in rat plasma by high performance liquid chromatography method and its application to pharmacokinetics studies.

    PubMed

    Chen, QiuHong; Hou, ShiXiang; Zheng, Jia; Bi, YueQi; Li, YuanBo; Yang, XiaoJiao; Cai, Zheng; Song, XiangRong

    2007-10-15

    A sensitive and reproducible high performance liquid chromatography method with UV detection was described for the determination of aesculin in rat plasma. After deproteinization by methanol using metronidazole as internal standard (I.S.), solutes were evaporated to dryness at 40 degrees C under a gentle stream of nitrogen. The residue was reconstituted in 100 microl of mobile phase and a volume of 20 microl was injected into the HPLC for analysis. Solutes were separated on a Diamonsil C18 column (250 mm x 4.6 mm i.d., 5 microm particle size, Dikma) protected by a ODS guard column (10 mm x 4.0 mm i.d., 5 microm particle size), using acetonitrile-0.1% triethylamine solution (adjusted to pH 3.0 using phosphoric acid) (10:90, v/v) as mobile phase (flow-rate 1.0 ml/min), and wavelength of the UV detector was set at 338 nm. No interference from any endogenous substances was observed during the elution of aesculin and internal standard (I.S., metronidazole). The retention times for I.S and aesculin were 10.4 and 12.4 min, respectively. The limit of quantification was evaluated to be 57.4 ng/ml and the limit of detection was 24.0 ng/ml. The method was used in the study of pharmacokinetics of aesculin after intraperitoneal injection (i.p.) administration in rats.

  19. Phentermine interference and high L-methamphetamine concentration problems in GC-EI-MS SIM Analyses of R-(-)-α-methoxy-α-(trifluoromethyl)phenylacetyl chloride-derivatized amphetamines and methamphetamines†.

    PubMed

    Hamilton, Theron J; Qui, Harry Z; Dozier, Katherine V R; Fuller, Zachary J

    2014-09-01

    In order to achieve chromatographic separation, urine samples shown to be initially positive for amphetamines and methamphetamines in US Department of Defense immunoassays are derivatized with R-(-)-α-methoxy-α-(trifluoromethyl)phenylacetyl chloride (R-(-)-MTPA) prior to gas chromatography-electron impact-mass spectrometry (GC-EI-MS) analysis. Phentermine, a member of the phenethylamine class of drugs and a common appetite suppressant, interferes with GC-EI-MS assays of R-(-)-MTPA-derivatized d-amphetamine, degrading the chromatography of the internal standard and analyte ions and skewing concentration calculations. Additionally, when specimens with high concentrations of l-methamphetamine are derivatized with R-(-)-MTPA, signal peaks have the potential to be misidentified by integration software as d-methamphetamine. We have found that replacing R-(-) MTPA with (S)-(+)-α-methoxy-α-(trifluoromethyl)phenylacetyl chloride reduces phentermine interference problems related to internal standard chromatography, reduces the possibility of concentrated l-methamphetamine peaks being misidentified by integration software, improves resolution of d-methamphetamine in the presence of high l-methamphetamine concentrations, and is a cost-neutral change that can be applied to current amphetamines GC-EI-MS methods without the need for method modification. Published by Oxford University Press 2014. This work is written by (a) US Government employee(s) and is in the public domain in the US.

  20. Rapid amino acid quantitation with pre-column derivatization; ultra-performance reverse phase liquid chromatography and single quadrupole mass spectrometry.

    PubMed

    Pretorius, Carel J; McWhinney, Brett C; Sipinkoski, Bilyana; Wilce, Alice; Cox, David; McWhinney, Avis; Ungerer, Jacobus P J

    2018-03-01

    We optimized a quantitative amino acid method with pre-column derivatization, norvaline (nva) internal standard and reverse phase ultra-performance liquid chromatography by replacing the ultraviolet detector with a single quadrupole mass spectrometer (MS nva ). We used 13 C 15 N isotopically labeled amino acid internal standards and a C18 column with 1.6μm particles to optimize the chromatography and to confirm separation of isobaric compounds (MS lis ). We compared the analytical performance of MS nva with MS lis and the original method (UV nva ) with clinical samples. The chromatography time per sample of MS nva was 8min, detection capabilities were <1μmol/L for most components, intermediate imprecisions at low concentrations were <10% and there was negligible carryover. MS nva was linear up to a total amino acid concentration in a sample of approximately 9500μmol/L. The agreements between most individual amino acids were satisfactory compared to UV nva with the latter prone to outliers and suboptimal quantitation of urinary arginine, aspartate, glutamate and methionine. MS nva reliably detected argnininosuccinate, β-alanine, citrulline and cysteine-s-sulfate. MS nva resulted in a more than fivefold increase in operational efficiency with accurate detection of amino acids and metabolic intermediates in clinical samples. Crown Copyright © 2017. Published by Elsevier B.V. All rights reserved.

  1. Simultaneous quantification of fentanyl, sufentanil, cefazolin, doxapram and keto-doxapram in plasma using liquid chromatography - tandem mass spectrometry.

    PubMed

    Flint, Robert B; Bahmany, Soma; van der Nagel, Bart C H; Koch, Birgit C P

    2018-05-16

    A simple and specific UPLC-MS/MS method was developed and validated for simultaneous quantification of fentanyl, sufentanil, cefazolin, doxapram and its active metabolite keto-doxapram. The internal standard was fentanyl-d5 for all analytes. Chromatographic separation was achieved with a reversed phase Acquity UPLC HSS T3 column with a run-time of only 5.0 minutes per injected sample. Gradient elution was performed with a mobile phase consisting of ammonium acetate, formic acid in Milli-Q ultrapure water or in methanol with a total flow rate of 0.4 mL minute -1 . A plasma volume of only 50 μL was required to achieve both adequate accuracy and precision. Calibration curves of all 5 analytes were linear. All analytes were stable for at least 48 hours in the autosampler. The method was validated according to US Food and Drug Administration guidelines. This method allows quantification of fentanyl, sufentanil, cefazolin, doxapram and keto-doxapram, which serves purposes for research, as well as therapeutic drug monitoring, if applicable. The strength of this method is the combination of a small sample volume, a short run-time, a deuterated internal standard, an easy sample preparation method and the ability to simultaneously quantify all analytes in one run. This article is protected by copyright. All rights reserved.

  2. Clinical, aetiological, anatomical and pathological classification (CEAP): gold standard and limits.

    PubMed

    Rabe, E; Pannier, F

    2012-03-01

    The first CEAP (clinical, aetiological, anatomical and pathological elements) consensus document was published after a consensus conference of the American Venous Forum, held at the sixth annual meeting of the AVF in February 1994 in Maui, Hawaii. In the following years the CEAP classification was published in many international journals and books which has led to widespread international use of the CEAP classification since 1995. The aim of this paper is to review the benefits and limits of CEAP from the available literature. In an actual Medline analysis with the keywords 'CEAP' and 'venous insufficiency', 266 publications using the CEAP classification in venous diseases are available. The CEAP classification was accepted in the venous community and used in scientific publications, but in most of the cases only the clinical classification was used. Limitations of the first version including a lack of clear definition of clinical signs led to a revised version. The CEAP classification is the gold standard of classification of chronic venous disorders today. Nevertheless for proper use some facts have to be taken into account: the CEAP classification is not a severity classification, C2 summarizes all kinds of varicose veins, in C3 it may be difficult to separate venous and other reasons for oedema, and corona phlebectatica is not included in the classification. Further revisions of the CEAP classification may help to overcome the still-existing deficits.

  3. A critical overview of definitions and determination techniques of the internal resistance using lithium-ion, lead-acid, nickel metal-hydride batteries and electrochemical double-layer capacitors as examples

    NASA Astrophysics Data System (ADS)

    Piłatowicz, Grzegorz; Marongiu, Andrea; Drillkens, Julia; Sinhuber, Philipp; Sauer, Dirk Uwe

    2015-11-01

    The internal resistance (Ri) is one of the key parameters that determine the current state of electrochemical storage systems (ESS). It is crucial for estimating cranking capability in conventional cars, available power in modern hybrid and electric vehicles and for determining commonly used factors such as state-of-health (SoH) and state-of-function (SoF). However, ESS are complex and non-linear systems. Their Ri depends on many parameters such as current rate, temperature, SoH and state-of-charge (SoC). It is also a fact that no standardized methodologies exist and many different definitions and ways of Ri determination are being used. Nevertheless, in many cases authors are not aware of the consequences that occur when different Ri definitions are being used, such as possible misinterpretations, doubtful comparisons and false figures of merit. This paper focuses on an application-oriented separation between various Ri definitions and highlights the differences between them. The investigation was based on the following technologies: lead-acid, lithium-ion and nickel metal-hydride batteries as well as electrochemical double-layer capacitors. It is not the target of this paper to provide a standardized definition of Ri but to give researchers, engineers and manufacturers a possibility to understand what the term Ri means in their own work.

  4. A quantitative LC-MS/MS method for simultaneous determination of cocaine and its metabolites in whole blood

    PubMed Central

    Chen, Xiabin; Zheng, Xirong; Ding, Kai; Zhou, Ziyuan; Zhan, Chang-Guo; Zheng, Fang

    2016-01-01

    As new metabolic pathways of cocaine were recently identified, a high performance liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously determine cocaine and nine cocaine-related metabolites in whole blood samples. One-step solid phase extraction was used to extract all of the ten compounds and corresponding internal standards from blood samples. All compounds and internal standards extracted were separated on an Atlantis T3 (100Å, 3 µm, 2.1 mm × 150 mm I.D) column and detected in positive ion and high sensitivity mode with multiple reaction monitoring. This method was validated for its sensitivity, linearity, specificity, accuracy, precision, recovery, and stability. All of the ten compounds were quantifiable ranging from the lower limit of quantification (LLOQs) of ~10 nM (1.9–3.2 ng/ml) to ~1000 nM (190–320 ng/ml) without any interfering substance. Accuracy and precision were determined, and both of them were within the acceptance criteria of the United States (US) Food and Drug Administration (FDA) and European Medicines Agency (EMA) guidelines. The recovery was above 66.7% for all compounds. Stability tests demonstrated the stability of compounds under different storage conditions in whole blood samples. The method was successfully applied to a pharmacokinetic study with co-administration of cocaine and alcohol in rats. PMID:27923200

  5. Validated high-performance liquid chromatographic method utilizing solid-phase extraction for the simultaneous determination of naringenin and hesperetin in human plasma.

    PubMed

    Kanaze, Feras Imad; Kokkalou, Eugene; Georgarakis, Manolis; Niopas, Ioannis

    2004-03-05

    Naringenin and hesperetin, the aglycones of the flavanone glucosides naringin and hesperidin occur naturally in citrus fruits. They exert a variety of pharmacological effects such as antioxidant, blood lipid-lowering, anticarcinogenic and inhibit selected cytochrome P-450 enzymes resulting in drug interactions. A specific, sensitive, precise, and accurate solid-phase extraction high-performance liquid chromatographic (HPLC) assay for the simultaneous determination of naringenin and hesperetin in human plasma was developed and validated. After addition of 7-ethoxycoumarin as internal standard, plasma samples were incubated with beta-glucuronidase/sulphatase, and the analytes were isolated from plasma by solid-phase extraction using C(18) cartridges and separated on a C(8) reversed phase column with methanol/water/acetic acid (40:58:2, v/v/v) as the eluent at 45 degrees C. The method was linear in the 10-300 ng/ml concentration range for both naringenin and hesperetin (r>0.999). Recovery for naringenin, hesperetin and internal standard was greater than 76.7%. Intra- and inter-day precision for naringenin ranged from 1.4 to 4.2% and from 1.9 to 5.2%, respectively, and for hesperetin ranged from 1.3 to 4.1% and from 1.7 to 5.1%, respectively. Accuracy was better than 91.5 and 91.3% for naringenin and hesperetin, respectively.

  6. Porting and redesign of Geotool software system to Qt

    NASA Astrophysics Data System (ADS)

    Miljanovic Tamarit, V.; Carneiro, L.; Henson, I. H.; Tomuta, E.

    2016-12-01

    Geotool is a software system that allows a user to interactively display and process seismoacoustic data from International Monitoring System (IMS) station. Geotool can be used to perform a number of analysis and review tasks, including data I/O, waveform filtering, quality control, component rotation, amplitude and arrival measurement and review, array beamforming, correlation, Fourier analysis, FK analysis, event review and location, particle motion visualization, polarization analysis, instrument response convolution/deconvolution, real-time display, signal to noise measurement, spectrogram, and travel time model display. The Geotool program was originally written in C using the X11/Xt/Motif libraries for graphics. It was later ported to C++. Now the program is being ported to the Qt graphics system to be more compatible with the other software in the International Data Centre (IDC). Along with this port, a redesign of the architecture is underway to achieve a separation between user interface, control, and data model elements, in line with design patterns such as Model-View-Controller. Qt is a cross-platform application framework that will allow geotool to easily run on Linux, Mac, and Windows. The Qt environment includes modern libraries and user interfaces for standard utilities such as file and database access, printing, and inter-process communications. The Qt Widgets for Technical Applications library (QWT) provides tools for displaying standard data analysis graphics.

  7. High performance liquid chromatography with UV detection for the simultaneous determination of sympathomimetic amines using 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride as a label.

    PubMed

    Kaddoumi, A; Kubota, A; Nakashima, M N; Takahashi, M; Nakashima, K

    2001-10-01

    A high performance liquid chromatographic method has been developed for the simultaneous determination of (+/-) fenfluramine (Fen) and phentermine (Phen) in addition to three other sympathomimetic amines-ephedrine (E), norephedrine (NE) and 2-phenylethylamine (2-PEA), using cyclohexylamine (CX) as an internal standard in plasma. The compounds were derivatized with 4-(4,5-diphenyl-1H-imidazole-2-yl)benzoyl chloride (DIB-Cl) to give the DIB-derivatives. The derivatives were then separated using an isocratic HPLC system with UV detection. The limits of detection for Fen, Phen, E, NE and 2-PEA in plasma ranged from 0.32 to 22.9 pmol on column at a signal-to-noise ratio of 3. The recoveries following alkaline extraction from plasma samples of known concentrations were found to be more than 94% for the studied compounds. This method might be useful for the screening of the studied sympathomimetic amines in human plasma samples in forensic as well as toxicological studies. Furthermore, the developed method was modified for the simultaneous determination of Fen and Phen in human and rat plasma using fluoxetine as an internal standard. The methods are reproducible and precise. Finally, the two drugs were administered intraperitoneally to rats in combination, and their plasma levels over the investigated time course were successfully determined. Copyright 2001 John Wiley & Sons, Ltd.

  8. Validation of an LC-MS/MS Method for Urinary Lactulose and Mannitol Quantification: Results in Patients with Irritable Bowel Syndrome.

    PubMed

    Gervasoni, Jacopo; Schiattarella, Arcangelo; Giorgio, Valentina; Primiano, Aniello; Russo, Consuelo; Tesori, Valentina; Scaldaferri, Franco; Urbani, Andrea; Zuppi, Cecilia; Persichilli, Silvia

    2016-01-01

    Aim . Lactulose/mannitol ratio is used to assess intestinal barrier function. Aim of this work was to develop a robust and rapid method for the analysis of lactulose and mannitol in urine by liquid chromatography coupled to tandem mass spectrometry. Lactulose/mannitol ratio has been measured in pediatric patients suffering from irritable bowel syndrome. Methods . Calibration curves and raffinose, used as internal standard, were prepared in water : acetonitrile 20 : 80. Fifty μ L of urine sample was added to 450  μ L of internal standard solution. The chromatographic separation was performed using a Luna NH 2 column operating at a flow rate of 200  μ L/min and eluted with a linear gradient from 20% to 80% water in acetonitrile. Total run time is 9 minutes. The mass spectrometry operates in electrospray negative mode. Method was fully validated according to European Medicine Agency guidelines. Results and Conclusions . Linearity ranged from 10 to 1000 mg/L for mannitol and 2.5 to 1000 mg/L for lactulose. Imprecision in intra- and interassay was lower than 15% for both analytes. Accuracy was higher than 85%. Lactulose/mannitol ratio in pediatric patients is significantly higher than that measured in controls. The presented method, rapid and sensitive, is suitable in a clinical laboratory.

  9. Detector Outline Document for the Fourth Concept Detector ("4th") at the International Linear Collider

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

    Barbareschi, Daniele; et al.

    We describe a general purpose detector ( "Fourth Concept") at the International Linear Collider (ILC) that can measure with high precision all the fundamental fermions and bosons of the standard model, and thereby access all known physics processes. The 4th concept consists of four basic subsystems: a pixel vertex detector for high precision vertex definitions, impact parameter tagging and near-beam occupancy reduction; a Time Projection Chamber for robust pattern recognition augmented with three high-precision pad rows for precision momentum measurement; a high precision multiple-readout fiber calorimeter, complemented with an EM dual-readout crystal calorimeter, for the energy measurement of hadrons, jets,more » electrons, photons, missing momentum, and the tagging of muons; and, an iron-free dual-solenoid muon system for the inverse direction bending of muons in a gas volume to achieve high acceptance and good muon momentum resolution. The pixel vertex chamber, TPC and calorimeter are inside the solenoidal magnetic field. All four subsytems separately achieve the important scientific goal to be 2-to-10 times better than the already excellent LEP detectors, ALEPH, DELPHI, L3 and OPAL. All four basic subsystems contribute to the identification of standard model partons, some in unique ways, such that consequent physics studies are cogent. As an integrated detector concept, we achieve comprehensive physics capabilities that puts all conceivable physics at the ILC within reach.« less

  10. A new LC-MS/MS bioanalytical method for atenolol in human plasma and milk.

    PubMed

    Phyo Lwin, Ei Mon; Gerber, Cobus; Song, Yunmei; Leggett, Catherine; Ritchie, Usha; Turner, Sean; Garg, Sanjay

    2017-04-01

    A new sensitive LC-MS/MS method for the quantification of atenolol in human plasma and milk has been developed for clinical lactation studies. Atenolol and the internal standard, phenazone, were extracted from biological matrices by protein precipitation. A Phenomenex ® C-18 column and gradient chromatographic conditions were used for separation of the analyte, followed by detection with MS. Stability of samples was confirmed for atenolol in human plasma and milk for up to 3 months. Linearity range of 1-800 ng/ml (r 2 = 0.9995), the precision within 15% CV and the recovery of the analyte (80-100% range) were achieved. A new validated analytical method for atenolol in plasma and milk was developed.

  11. Identification and measurement of pesticide contaminants in food products by electron impact GC/MS

    NASA Astrophysics Data System (ADS)

    Tusa, Florina; Moldovan, Zaharie; Vlassa, Mircea

    2009-08-01

    The paper concern is determination of eight pesticides in food products samples. The target compounds are: Lindane, Heptachlor, Aldrin, o,p-DDE, Dieldrin, Endrin, p,p'-DDT, and Methoxychlor. The compounds quantities were performed from chromatographic area obtained in full scan GC/MS mode after baseline separation and by comparation with surrogate internal standard area (Diphenylamine). The samples were concentrated by extraction with organic solvents (acetone) by Solid-Liquid Extraction (SLE) procedures the recovery factors being better than 80% except for Heptachlors. The coefficient of correlation of detector response function was better than 0.913 and LOQ under 0.015 μg/g. The method enables to determine pesticides at low μg/g in food supplements.

  12. Simultaneous determination of chloroquine and its three metabolites in human plasma, whole blood and urine by ion-pair high-performance liquid chromatography.

    PubMed

    Houzé, P; de Reynies, A; Baud, F J; Benatar, M F; Pays, M

    1992-02-14

    A method was developed for the separation and measurement of chloroquine and three metabolites (desethylchloroquine, bisdesethylchloroquine and 4-amino-7-chloroquinoline) in biological samples by ion-pair high-performance liquid chromatography with UV detection. The method uses 2,3-diaminoaphthalene as an internal standard and provides a limit of detection between 1 and 2 ng/ml for chloroquine and its metabolites. The assay was linear in the range 12.5-250 ng/ml and the analytical recovery and reproducibility were sufficient. The assay was applied to the analysis of biological samples from a patient undergoing chloroquine chemoprophylaxis and a patient who had ingested chloroquine in a suicide attempt.

  13. Analysis of 6-mercaptopurine in human plasma with a high-performance liquid chromatographic method including post-column derivatization and fluorimetric detection.

    PubMed

    Jonkers, R E; Oosterhuis, B; ten Berge, R J; van Boxtel, C J

    1982-12-10

    A relatively simple assay with improved reliability and sensitivity for measuring levels of 6-mercaptopurine in human plasma is presented. After extraction of the compound and the added internal standard with phenyl mercury acetate, samples were separated by ion-pair reversed-phase high-performance liquid chromatography. On-line the analytes were oxidized to fluorescent products and detected in a flow-fluorimeter. The within-day coefficient of variation was 3.8% at a concentration of 25 ng/ml. The lower detection limit was 2 ng/ml when 1.0 ml of plasma was used. Mercaptopurine concentration versus time curves of two subjects after a single oral dose of azathioprine are shown.

  14. Coded Modulation in C and MATLAB

    NASA Technical Reports Server (NTRS)

    Hamkins, Jon; Andrews, Kenneth S.

    2011-01-01

    This software, written separately in C and MATLAB as stand-alone packages with equivalent functionality, implements encoders and decoders for a set of nine error-correcting codes and modulators and demodulators for five modulation types. The software can be used as a single program to simulate the performance of such coded modulation. The error-correcting codes implemented are the nine accumulate repeat-4 jagged accumulate (AR4JA) low-density parity-check (LDPC) codes, which have been approved for international standardization by the Consultative Committee for Space Data Systems, and which are scheduled to fly on a series of NASA missions in the Constellation Program. The software implements the encoder and decoder functions, and contains compressed versions of generator and parity-check matrices used in these operations.

  15. Application of Internal Standard Method for Several 3d-Transition Metallic Elements in Flame Atomic Absorption Spectrometry Using a Multi-wavelength High-resolution Spectrometer.

    PubMed

    Toya, Yusuke; Itagaki, Toshiko; Wagatsuma, Kazuaki

    2017-01-01

    We investigated a simultaneous internal standard method in flame atomic absorption spectrometry (FAAS), in order to better the analytical precision of 3d-transition metals contained in steel materials. For this purpose, a new spectrometer system for FAAS, comprising a bright xenon lamp as the primary radiation source and a high-resolution Echelle monochromator, was employed to measure several absorption lines at a wavelength width of ca. 0.3 nm at the same time, which enables the absorbances of an analytical line and also an internal standard line to be estimated. In considering several criteria for selecting an internal standard element and the absorption line, it could be suggested that platinum-group elements: ruthenium, rhodium, or palladium, were suitable for an internal standard element to determine the 3d-transition metal elements, such as titanium, iron, and nickel, by measuring an appropriate pair of these absorption lines simultaneously. Several variances of the absorption signal, such as a variation in aspirated amounts of sample solution and a short-period drift of the primary light source, would be corrected and thus reduced, when the absorbance ratio of the analytical line to the internal standard line was measured. In Ti-Pd, Ni-Rh, and Fe-Ru systems chosen as typical test samples, the repeatability of the signal respnses was investigated with/without the internal standard method, resulting in better precision when the internal standard method was applied in the FAAS with a nitrous oxide-acetylene flame rather than an air-acetylene flame.

  16. Quality assurance in military medical research and medical radiation accident management.

    PubMed

    Hotz, Mark E; Meineke, Viktor

    2012-08-01

    The provision of quality radiation-related medical diagnostic and therapeutic treatments cannot occur without the presence of robust quality assurance and standardization programs. Medical laboratory services are essential in patient treatment and must be able to meet the needs of all patients and the clinical personnel responsible for the medical care of these patients. Clinical personnel involved in patient care must embody the quality assurance process in daily work to ensure program sustainability. In conformance with the German Federal Government's concept for modern departmental research, the international standard ISO 9001, one of the relevant standards of the International Organization for Standardization (ISO), is applied in quality assurance in military medical research. By its holistic approach, this internationally accepted standard provides an excellent basis for establishing a modern quality management system in line with international standards. Furthermore, this standard can serve as a sound basis for the further development of an already established quality management system when additional standards shall apply, as for instance in reference laboratories or medical laboratories. Besides quality assurance, a military medical facility must manage additional risk events in the context of early recognition/detection of health risks of military personnel on deployment in order to be able to take appropriate preventive and protective measures; for instance, with medical radiation accident management. The international standard ISO 31000:2009 can serve as a guideline for establishing risk management. Clear organizational structures and defined work processes are required when individual laboratory units seek accreditation according to specific laboratory standards. Furthermore, international efforts to develop health laboratory standards must be reinforced that support sustainable quality assurance, as in the exchange and comparison of test results within the scope of external quality assurance, but also in the exchange of special diagnosis data among international research networks. In summary, the acknowledged standard for a quality management system to ensure quality assurance is the very generic standard ISO 9001.Health Phys. 103(2):221-225; 2012.

  17. Precolumn derivatization followed by liquid chromatographic separation and determination of tramiprosate in rat plasma by fluorescence detector: application to pharmacokinetics.

    PubMed

    Rao, R Nageswara; Maurya, Pawan K; Shinde, Dhananjay D; Khalid, Sara

    2011-05-15

    Alzheimer disease (AD) is characterized pathologically by extracellular amyloid deposits composed of amyloid β (Aβ) protein. A simple and rapid method using HPLC with fluorescence detector was developed and validated for determination of tramiprosate in rat plasma. Pre-column derivatization of the deproteinized rat plasma was carried out using o-phthaldialdehyde (OPA) as a fluorescent reagent in presence of 3-mercaptopropionic acid. The liquid chromatographic separation was achieved on a Kromasil C18 column using methanol:acetonitrile: 20 mM phosphate buffer pH 7.5 (8.0:17.5:74.5 v/v/v) as a mobile phase in an isocratic elution mode. The eluents were monitored by a fluorescence detector set at 330 and 450 nm of excitation and emission wavelength respectively. Vigabatrin was used as an internal standard. The method was linear within the range 30.0-1000.0 ng/mL. Design of experiments (DOE) was used to evaluate the robustness of the method. The developed method was applied to study the pharmacokinetics of tramiprosate in rats. Copyright © 2011. Published by Elsevier B.V.

  18. Preconcentration and determination of rare-earth elements in iron-rich water samples by extraction chromatography and plasma source mass spectrometry (ICP-MS).

    PubMed

    Hernández González, Carolina; Cabezas, Alberto J Quejido; Díaz, Marta Fernández

    2005-11-15

    A 100-fold preconcentration procedure based on rare-earth elements (REEs) separation from water samples with an extraction chromatographic column has been developed. The separation of REEs from matrix elements (mainly Fe, alkaline and alkaline-earth elements) in water samples was performed loading the samples, previously acidified to pH 2.0 with HNO(3), in a 2ml column preconditioned with 20ml 0.01M HNO(3). Subsequently, REEs were quantitatively eluted with 20ml 7M HNO(3). This solution was evaporated to dryness and the final residue was dissolved in 10ml 2% HNO(3) containing 1mugl(-1) of cesium used as internal standard. The solution was directly analysed by inductively coupled plasma mass spectrometry (ICP-MS), using ultrasonic nebulization, obtaining quantification limits ranging from 0.05 to 0.10 ngl(-1). The proposed method has been applied to granitic waters running through fracture fillings coated by iron and manganese oxy-hydroxides in the area of the Ratones (Cáceres, Spain) old uranium mine.

  19. Quantitative analysis of retinoids in biological fluids by high-performance liquid chromatography using column switching. I. Determination of isotretinoin and tretinoin and their 4-oxo metabolites in plasma.

    PubMed

    Wyss, R; Bucheli, F

    1988-02-26

    A fully automated gradient high-performance liquid chromatographic method for the determination of isotretinoin, tretinoin and their 4-oxo metabolites in plasma was developed, using the column-switching technique. After dilution with an internal standard solution containing 20% acetonitrile, 0.5 ml of the sample was injected onto a precolumn (17 X 4.6 mm I.D.), filled with C18 Corasil 37-53 micron. Proteins and polar plasma components were washed out using 1% ammonium acetate-acetonitrile (9:1, v/v) as mobile phase 1. After valve switching, the retained components were transferred to the analytical column in the backflush mode, separated by gradient elution and detected at 360 nm by UV detection. Using two coupled reversed-phase columns (125 mm long), the separation of cis and trans isomers was possible, and all four compounds could be quantified down to 2 ng/ml of plasma. The inter-assay precision in the concentration range 20-100 ng/ml was between 1.0 and 4.7% for all compounds.

  20. [Determination of ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride in maxingshigan decoction by CE].

    PubMed

    Yu, Li-ping; Wang, Xiao-ke; Luo, Jia-bo

    2011-04-01

    To establish the method for determination of ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride in maxingshigan decoction by capillary electrophoresis. The separation was performed on a fused silica capillary of 60 cm x 55 microcrpm ID (52 cm of effective length). 60 mmol/L NaB4O7 + 10% (V/V) CH3OH (pH 9.0) was selected as the running buffer. The separation voltage was 12 kV. The samples was injected by gravity (10 s, 15 cm). The detection wavelength was 210 nm and berberine hydrochloride was the internal standard. The linear range of determination for ephedrine hydrochloride, pseudoephedrine hydrochloride and methylephedrine hydrochloride were 20.0-160.0 microg/mL (r = 0.9999), 7.5-60.0 microg/mL (r = 0.9991) and 2.0-10.0 microg/mL (r = 0.9993). The average recoveries were 98.0%, 97.0% and 97.8%, the precisions of the method were 2.31%, 2.21% and 2.00% (n=6), respectively. The method is convenient, rapid and accurate for the quality control of maxingshigan decoction.

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