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Sample records for analytical methods validation

  1. Validation of analytical methods

    Directory of Open Access Journals (Sweden)

    Xavier Rius, F.

    2002-03-01

    Full Text Available In this paper we shall discuss the concept of method validation, describe the various elements and explain its close relationship with fitness for purpose. Method validation is based on the assumption that a series of requirements are fulfilled and we shall explain how these requirements are selected, the way in which evidence is supplied and what work has to be carried out in the laboratory. The basic principles of method validation and the different ways to validate a methodology, by inter-laboratory comparison or performing an in-house validation, are also described.En este artículo se discute el concepto de validación del método, se describen los elementos que la componen y se explica la fuerte relación entre la validación y las características de ajuste. El método de validación se basa en el cumplimiento de una serie de requerimientos, se explica como seleccionar esos requerimientos, la forma en que se suministran evidencias, y que trabajo se debe llevar a cabo en el laboratorio. También se describen, los principios básicos del método de validación y los diferentes caminos para validar una metodología, tanto en la comparación entre laboratorios o como cuando se lleva a cabo una validación dentro del laboratorio.

  2. ANALYTICAL METHOD VALIDATION: AN UPDATED REVIEW

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    G. Lavanya, M. Sunil, M.M. Eswarudu*, M. C. Eswaraiah, K. Harisudha and B. Naga Spandana

    2013-04-01

    Full Text Available ABSTRACT: The development of sound Analytical method(s is of supreme importance during the process of drug discovery, release to market and development, culminating in a marketing approval. The objective of this paper is to review the method development, optimize and validation of the method for the drug product from the developmental stage of the formulation to commercial batch of the product. Method development for the interested component in finished product or in process tests and the sample preparation of drug product and to provide practical approaches for determining selectivity, specificity, limit of detection, limit of quantitation, linearity, range accuracy, precision, recovery solution stability, ruggedness, and robustness of liquid chromatographic methods to support the Routine, in process and stability analysis.

  3. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR DIPYRIDAMOLE

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    SURESH KUMAR,LATIF D.JAMADAR, KRIS KRISHNAMURTHY BHAT, JAGDISH P.C, SHRIRAM PATHAK

    2013-10-01

    Full Text Available A sensitive, specific, precise and cost effective High Performance Liquid Chromatographic method of analysis for dipyridamole in presence of its degradation products is developed and validated. The method employed Targa C8 column i.e., (250 X 4.6 mm 5 μm particle size column as stationary phase. The mobile phase consists of acetonitrile and pH3.0 buffer in the ratio of 35:65 %. It is pumped through the chromatographic system at a flow rate of 1.2 ml/min. The UV detector is operated at 282 nm. This system was found to give good resolution between dipyridamole and its degradation products. Method was validated as per ICH guidelines

  4. Oxcarbazepine: validation and application of an analytical method

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    Paula Cristina Rezende Enéas

    2010-06-01

    Full Text Available Oxcarbazepine (OXC is an important anticonvulsant and mood stabilizing drug. A pharmacopoeial monograph for OXC is not yet available and therefore the development and validation of a new analytical method for quantification of this drug is essential. In the present study, a UV spectrophotometric method for the determination of OXC was developed. The various parameters, such as linearity, precision, accuracy and specificity, were studied according to International Conference on Harmonization Guidelines. Batches of 150 mg OXC capsules were prepared and analyzed using the validated UV method. The formulations were also evaluated for parameters including drug-excipient compatibility, flowability, uniformity of weight, disintegration time, assay, uniformity of content and the amount of drug dissolved during the first hour.Oxcarbazepina (OXC é um fármaco anticonvulsivante e estabilizante do humor. O desenvolvimento e validação de método analítico para quantificação da OXC são de fundamental importância devido à ausência de monografias farmacopéicas oficiais para esse fármaco. Nesse trabalho, um método espectrofotométrico UV para determinação da OXC foi desenvolvido. O método proposto foi validado seguindo os parâmetros de linearidade, precisão, exatidão e especificidade de acordo com as normas da Conferência Internacional de Harmonização. Cápsulas de OXC 150 mg foram preparadas e analisadas utilizando-se o método analítico validado. As formulações foram avaliadas com relação à compatibilidade fármaco-excipientes, fluidez, determinação de peso, tempo de desintegração, doseamento, uniformidade de conteúdo e quantidade do fármaco dissolvido após 60 minutos.

  5. Analytical Method Development & Validation for Related Substances Method of Busulfan Injection by Ion Chromatography Method

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    Rewaria S

    2013-05-01

    Full Text Available A new simple, accurate, precise and reproducible Ion chromatography method has been developed forthe estimation of Methane sulfonic acid in Busulfan injectable dosage. The method which is developedis also validated in complete compliance with the current regulatory guidelines by using well developedanalytical method validation techniques and tools which comprises with the analytical method validationparameters like Linearity, LOD and LOQ determination, Accuracy, Method precision, Specificity,System suitability, Robustness, Ruggedness etc. by adopting the current method the linearity obtained isnear to 0.999 and thus this shows that the method is capable to give a good detector response, therecovery calculated was within the range of 85% to 115% of the specification limits.

  6. Methodology for the validation of analytical methods involved in uniformity of dosage units tests.

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    Rozet, E; Ziemons, E; Marini, R D; Boulanger, B; Hubert, Ph

    2013-01-14

    Validation of analytical methods is required prior to their routine use. In addition, the current implementation of the Quality by Design (QbD) framework in the pharmaceutical industries aims at improving the quality of the end products starting from its early design stage. However, no regulatory guideline or none of the published methodologies to assess method validation propose decision methodologies that effectively take into account the final purpose of developed analytical methods. In this work a solution is proposed for the specific case of validating analytical methods involved in the assessment of the content uniformity or uniformity of dosage units of a batch of pharmaceutical drug products as proposed in the European or US pharmacopoeias. This methodology uses statistical tolerance intervals as decision tools. Moreover it adequately defines the Analytical Target Profile of analytical methods in order to obtain analytical methods that allow to make correct decisions about Content uniformity or uniformity of dosage units with high probability. The applicability of the proposed methodology is further illustrated using an HPLC-UV assay as well as a near infra-red spectrophotometric method.

  7. Analytical Quality by Design Approach to Test Method Development and Validation in Drug Substance Manufacturing

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    N. V. V. S. S. Raman

    2015-01-01

    Full Text Available Pharmaceutical industry has been emerging rapidly for the last decade by focusing on product Quality, Safety, and Efficacy. Pharmaceutical firms increased the number of product development by using scientific tools such as QbD (Quality by Design and PAT (Process Analytical Technology. ICH guidelines Q8 to Q11 have discussed QbD implementation in API synthetic process and formulation development. ICH Q11 guidelines clearly discussed QbD approach for API synthesis with examples. Generic companies are implementing QbD approach in formulation development and even it is mandatory for USFDA perspective. As of now there is no specific requirements for AQbD (Analytical Quality by Design and PAT in analytical development from all regulatory agencies. In this review, authors have discussed the implementation of QbD and AQbD simultaneously for API synthetic process and analytical methods development. AQbD key tools are identification of ATP (Analytical Target Profile, CQA (Critical Quality Attributes with risk assessment, Method Optimization and Development with DoE, MODR (method operable design region, Control Strategy, AQbD Method Validation, and Continuous Method Monitoring (CMM. Simultaneous implementation of QbD activities in synthetic and analytical development will provide the highest quality product by minimizing the risks and even it is very good input for PAT approach.

  8. Determination of proline in honey: comparison between official methods, optimization and validation of the analytical methodology.

    Science.gov (United States)

    Truzzi, Cristina; Annibaldi, Anna; Illuminati, Silvia; Finale, Carolina; Scarponi, Giuseppe

    2014-05-01

    The study compares official spectrophotometric methods for the determination of proline content in honey - those of the International Honey Commission (IHC) and the Association of Official Analytical Chemists (AOAC) - with the original Ough method. Results show that the extra time-consuming treatment stages added by the IHC method with respect to the Ough method are pointless. We demonstrate that the AOACs method proves to be the best in terms of accuracy and time saving. The optimized waiting time for the absorbance recording is set at 35min from the removal of reaction tubes from the boiling bath used in the sample treatment. The optimized method was validated in the matrix: linearity up to 1800mgL(-1), limit of detection 20mgL(-1), limit of quantification 61mgL(-1). The method was applied to 43 unifloral honey samples from the Marche region, Italy.

  9. Validation of multivariate classification methods using analytical fingerprints – concept and case study on organic feed for laying hens

    NARCIS (Netherlands)

    Alewijn, Martin; Voet, van der Hilko; Ruth, van Saskia

    2016-01-01

    Multivariate classification methods based on analytical fingerprints have found many applications in the food and feed area, but practical applications are still scarce due to a lack of a generally accepted validation procedure. This paper proposes a new approach for validation of this type of me

  10. Development and validation of HPLC analytical method for nepafenac in ophthalmic dosage form (suspension).

    Science.gov (United States)

    Usman, Shahnaz; Akram, Muhammad; Aziz, Asif; Ramesh, Venkat; Sarheed, Omar Abdulraheem

    2014-09-01

    The aim of the present study was to develop and validate an analytical method for the estimation of nepafenac as a raw material as well as in dosage form (suspension) by using reverse phase high performance liquid chromatographic (RP-HPLC). The target was to obtain an easy, rapid, reproducible as well as a rugged method. The HPLC system that was used in the proposed study was LC-20AD liquid chromatograph equipped with SPD-20A UV-VIS detector. The separation was performed on C18 column which was attached with loop 20 β l. Elution was done at ambient temperature with a mobile phase consisting of acetonitrile: Water (40: 60v/v) at a flow rate of 1ml/min and at a wavelength of 254 nm. The proposed method was validated as per the ICH guidelines. The retention time for nepafenac was 7.49 minutes (% CV=0.0076). The percentage coefficient variation (CV) of six consecutive peak areas of injections was 0.34% with tailing factor 1.76. The peak area responses were linear within the concentration range of 0.078-20.0 βg/ml (R(2)=0.9993). The sensitivity of the method could be evaluated by limits of detection (LOD) (0.0195 β g/ml) and limits of quantitation (LOQ) (0.039 β g/ml). Nepafenac drug is s in its diluent that could see by intra-day (% CV =0.45-1.96) and inter-day variation (%CV=0.173-1.898%). The accuracy and recovery results of 80%, 100% and 120% were 97.40% to 102.10% with % CV of 0.3201% to 1.3496%. The robustness and ruggedness of the method are significantly broader and is reproducible. It could be used as a more convenient, efficient, easy and time saving method for the analysis of drug in raw material as well as in dosage form (ophthalmic suspension).

  11. Development and validation of analytical method for Naftopidil in human plasma by LC–MS/MS

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    Pritam S. Jain

    2015-09-01

    Full Text Available A highly sensitive and simple high-performance liquid chromatographic–tandem mass spectrometric (LC–MS-MS assay is developed and validated for the quantification of Naftopidil in human plasma. Naftopidil is extracted from human plasma by methyl tertiary butyl ether and analyzed using a reversed-phase gradient elution on a discovery C 18 5 μ (50 × 4.6 column. A methanol: 2 mM ammonium formate (90:10 as mobile phase, is used and detection was performed by MS using electrospray ionization in positive mode. Propranolol is used as the internal standard. The lower limits of quantification are 0.495 ng/mL. The calibration curves are linear over the concentration range of 0.495–200.577 ng/mL of plasma for each analyte. This novel LC–MS-MS method shows satisfactory accuracy and precision and is sufficiently sensitive for the performance of pharmacokinetic studies in humans.

  12. Occurrence of erythromycin residues in sheep milk. Validation of an analytical method.

    Science.gov (United States)

    García-Mayor, M A; Paniagua-González, G; Soledad-Rodríguez, B; Garcinuño-Martínez, R M; Fernández-Hernando, P; Durand-Alegría, J S

    2015-04-01

    The paper describes a new and selective analytical sample treatment for quantitative extraction and preconcentration of erythromycin in presence of other macrolide antibiotics in sheep milk samples. The methodology is based on the use of a molecular imprinted polymer (MIP) employed as solid phase extraction sorbent (MISPE). The synthesized material by bulk polymerization using erythromycin (ERY) as template was evaluated as solid phase extraction sorbent, in a novel sample treatment technique that can be coupled to high-performance liquid chromatography with diode-array detector (HPLC-DAD). MIP selectivity was studied for other macrolide antibiotics with similar structures, such as tylosin (TYL), spiramycin (SPI), josamycin (JOS), roxithromycin (ROX) and ivermectin (IVER) getting recoveries for these interferents lower than 35%, for all cases except for ROX, which recoveries were around 85%. The variables affecting the molecularly imprinted solid-phase extraction (MISPE) procedure were optimized to select the best conditions of selectivity and sensitivity to determine ERY at concentration levels established by EU legislation in sheep milk. Under the selected experimental conditions, quantification limit was 24.1 µg kg(-1). Recoveries were higher than 98%, with RSDs between 0.7% and 2%. The proposed MISPE-HPLC method was validated and successfully applied to ERY analysis in sheep milk samples.

  13. VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

    Energy Technology Data Exchange (ETDEWEB)

    Ekechukwu, A.

    2008-12-17

    This document proposes to provide a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers, and books reviewed is given in Appendix 1. Available validation documents and guides are listed in the appendix; each has a brief description of application and use. In the referenced sources, there are varying approaches to validation and varying descriptions of validation at different stages in method development. This discussion focuses on validation and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all documents were published in English.

  14. VALIDATION OF ANALYTICAL METHODS AND INSTRUMENTATION FOR BERYLLIUM MEASUREMENT: REVIEW AND SUMMARY OF AVAILABLE GUIDES, PROCEDURES, AND PROTOCOLS

    Energy Technology Data Exchange (ETDEWEB)

    Ekechukwu, A

    2009-05-27

    Method validation is the process of evaluating whether an analytical method is acceptable for its intended purpose. For pharmaceutical methods, guidelines from the United States Pharmacopeia (USP), International Conference on Harmonisation (ICH), and the United States Food and Drug Administration (USFDA) provide a framework for performing such valications. In general, methods for regulatory compliance must include studies on specificity, linearity, accuracy, precision, range, detection limit, quantitation limit, and robustness. Elements of these guidelines are readily adapted to the issue of validation for beryllium sampling and analysis. This document provides a listing of available sources which can be used to validate analytical methods and/or instrumentation for beryllium determination. A literature review was conducted of available standard methods and publications used for method validation and/or quality control. A comprehensive listing of the articles, papers and books reviewed is given in the Appendix. Available validation documents and guides are listed therein; each has a brief description of application and use. In the referenced sources, there are varying approches to validation and varying descriptions of the valication process at different stages in method development. This discussion focuses on valication and verification of fully developed methods and instrumentation that have been offered up for use or approval by other laboratories or official consensus bodies such as ASTM International, the International Standards Organization (ISO) and the Association of Official Analytical Chemists (AOAC). This review was conducted as part of a collaborative effort to investigate and improve the state of validation for measuring beryllium in the workplace and the environment. Documents and publications from the United States and Europe are included. Unless otherwise specified, all referenced documents were published in English.

  15. Development and validation of analytical methods for monomeric and oligomeric migrants from nylon 12 packaging materials.

    NARCIS (Netherlands)

    Stoffers, N.H.; Brandl, F.; Linssen, J.P.H.; Franz, R.

    2003-01-01

    Analytical methods for the determination of laurolactam-the monomer of nylon 12-as well as the cyclic dimer and trimer were established. High performance liquid chromatography using ultraviolet (HPLC-UV) and mass spectrometric detection (HPLC-MS) were both found suitable to identify and quantify mon

  16. Development and Validation of Analytical method for Lopinavir and Ritonavir by HPLC

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    R. Arun

    2013-06-01

    Full Text Available This paper describes the development and validation of the HPLC method (254nm for the quantitation of lopinavir and ritonavir in pure form and pharmaceutical formulations. The method showed to be linear (r2 > 0.999, precise (R.S.D. < 0.21%, accurate (recovery of 100.11% for lopinavir and 99.96% for ritonavir, specific and robust. Three batches of lopinavir and ritonavir tablets were assayed by the validated method. The lopinavir contents in the tablets varied from 99.87 to 100.52%, while ritonavir contents showed 99.61 to 100.57%.

  17. Analytical Method Development and Validation of Related Substance Method for Bortezomib for Injection 3.5 mg/Vial by RP-HPLC Method

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    Utage M

    2013-04-01

    Full Text Available An accurate, precise, simple and economical High Performance Liquid Chromatographic method for therelated substance determination of Bortezomib in its lyophilized dosage form has been developed. Themethod developed is Reverse Phase High Performance Liquid Chromatographic method using HypersilBDS C18 column (Length: 150mm, Diameter: 4.6mm, Particle size: 5μ with Gradient programmed anda simple Acetonitrile, Water and Formic acid in the ratio of 30:70:0.1 (v/v/v respectively as mobilephase A and Acetonitrile, Water and Formic acid in the ratio of 80:20:0.1 (v/v/v respectively. Themethod so developed was validated in compliance with the regulatory guidelines by using welldeveloped analytical method validation tool which comprises with the analytical method validationparameters like Linearity, Accuracy, Method precision, Specificity with forced degradation, Systemsuitability, Robustness, LOD, LOQ and Ruggedness. The results obtained were well within theacceptance criteria.

  18. Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material

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    Hisao Nishijo

    2011-09-01

    Full Text Available Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of reproducing reliable results during analysis. This method is fast (running time of 10 minutes, selective, accurate, precise and robust for the determination of the drug, with no observed interfering substances in the optimum wavelength. It could be concluded that this may be a routine method for quality control laboratories to certify the quality of Lamotrigine.Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of

  19. Analytical Method Validation of Selected Organochlorine Pesticides in Fortified Rice Using Gas Chromatography with Electron Capture Detector

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    Mutia Kusuma Wardani

    2014-01-01

    Full Text Available Gas chromatography with electron capture detector (GC-ECD has been validated for simultaneous determination of selected organochlorine pesticides namely heptachlor, endosulfan, dieldrin, dan p,p’-dichlorodiphenyltrichloroethane (p,p’-DDT using aldrin as standard internal. Some parameters for analytical method validation were evaluated, i.e. linearity, precision, sensitivity expressed with limit of detection and limit of quantification, and recovery. GC-ECD was linear for determination of these pesticides with r values ≥ 0.99. The values of LOD obtained were 2.50, 2.97, 1.61, and 2.54 ng/mL for heptachlor, endosulphan, dieldrin, and p,p’-DDT, respectively. Furthermore, the relative standard deviation (RSD values obtained for the assessment of analytical precision were lower than those required by Horwitz. Finally, the used GC-ECD method was accurate for determination of these organochlorine psticides in fortified rice samples which were indicated by the acceptable recovery percentages.

  20. Impurities in biogas - validation of analytical methods for siloxanes; Foeroreningar i biogas - validering av analysmetodik foer siloxaner

    Energy Technology Data Exchange (ETDEWEB)

    Arrhenius, Karine; Magnusson, Bertil; Sahlin, Eskil [SP Technical Research Institute of Sweden, Boraas (Sweden)

    2011-11-15

    Biogas produced from digester or landfill contains impurities which can be harmful for component that will be in contact with the biogas during its utilization. Among these, the siloxanes are often mentioned. During combustion, siloxanes are converted to silicon dioxide which accumulates on the heated surfaces in combustion equipment. Silicon dioxide is a solid compound and will remain in the engine and cause damages. Consequently, it is necessary to develop methods for the accurate determination of these compounds in biogases. In the first part of this report, a method for analysis of siloxanes in biogases was validated. The sampling was performed directly at the plant by drawing a small volume of biogas onto an adsorbent tube under a short period of time. These tubes were subsequently sent to the laboratory for analysis. The purpose of method validation is to demonstrate that the established method is fit for the purpose. This means that the method, as used by the laboratory generating the data, will provide data that meets a set of criteria concerning precision and accuracy. At the end, the uncertainty of the method was calculated. In the second part of this report, the validated method was applied to real samples collected in waste water treatment plants, co-digestion plants and plants digesting other wastes (agriculture waste). Results are presented at the end of this report. As expected, the biogases from waste water treatment plants contained largely higher concentrations of siloxanes than biogases from co-digestion plants and plants digesting agriculture wastes. The concentration of siloxanes in upgraded biogas regardless of which feedstock was digested and which upgrading technique was used was low.

  1. Analytical Method Development and Validation for Simultaneous Estimation of Clotrimazole and Tinidazole by RP-HPLC

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    Joshi S

    2015-12-01

    Full Text Available An isocratic reverse phase High Performance Liquid Chromatographic (RP-HPLC method was developed and validated for simultaneous determination of Clotrimazole and Tinidazole in combined pharmaceutical dosage form. The successful separation of Clotrimazole and Tinidazole was achieved using Purospher® C18 (250 mm x 4.6 mm i.d., 5 μm column, with mobile phase consisting Phosphate buffer (pH 3.5: Acetonitrile (45:55. The mobile phase flow rate was 1.0 ml/min and the detection wavelength was 240 nm. The developed RP-HPLC method was validated according to ICH guidelines with respect to linearity, accuracy, precision, specificity and robustness and also the LOD and LOQ values were determined.

  2. Validation of the Analytical Method for the Determination of Flavonoids in Broccoli

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    Tuszyńska Magdalena

    2014-09-01

    Full Text Available A simple, accurate and selective HPLC method was developed and validated for determination of quercetin and kaempferol, which are the main flavonols in broccoli. The separation was achieved on a reversed-phase C18 column using a mobile phase composed of methanol/water (60/40 and phosphoric acid 0.2% at a flow rate of 1.0 ml min-1. The detection was carried out on a DAD detector at 370 nm. This method was validated according to the requirements for new methods, which include selectivity, linearity, precision, accuracy, limit of detection and limit of quantitation. The current method demonstrates good linearity, with R2 > 0.99. The recovery is within 98.07-102.15% and 97.92-101.83% for quercetin and kaempferol, respectively. The method is selective, in that quercetin and kaempferol are well separated from other compounds of broccoli with good resolution. The low limit of detection and limit of quantitation of quercetin and kaempferol enable the detection and quantitation of these flavonoids in broccoli at low con–centrations.

  3. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR ESTIMATION OF CILNIDIPINE AND METOPROLOL SUCCINATE

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    Mo.Salauddin A Shaikh

    2015-07-01

    Full Text Available A simple, specific, accurate and precise reversed phase high performance liquid chromatographic method was developed and validated for the simultaneous estimation of Cilnidipine and Metoprolol Succinate, using a Cosmosil C18 (250 х 4.6 mm i.d. column and a mobile phase composed of 0.05M potassium dihydrogen phosphate buffer: Methanol (70:30 pH 3.5 adjusted with ophosphoric acid and at flow rate of 1.0 ml/min. The retention times of Cilnidipine and Metoprolol Succinate were found to be 3.493 min and 5.960 min, respectively. Linearity was established for Cilnidipine and Metoprolol Succinate in the range of 12.5-37.5 μg/ml and 2.5-7.5 μg/ml, respectively. The percentage recoveries of Cilnidipine and Metoprolol Succinate were found to be in the range of 100.13-100.40 % and 99.24-100.29 %, respectively. The correlation coefficients for both components were found to be 0.999. The developed methods were validated according to ICH guidelines and values of linearity, accuracy, precision and other analysis were found to be in good accordance with the prescribed values. This method can be successfully employed for simultaneous quantitative analysis of Cilnidipine and Metoprolol Succinate in its dosage form. The developed HPLC method was subjected to stability indicating studies for marketed formulation. Interfering peak from degraded products or solvent did not interfere with estimation of drugs and the developed method was found to be specific for estimation of Cilnidipine and Metoprolol Succinate.

  4. The role of validated analytical methods in JECFA drug assessments and evaluation for recommending MRLs.

    Science.gov (United States)

    Boison, Joe O

    2016-05-01

    The Joint Food and Agriculture Organization and World Health Organization (FAO/WHO) Expert Committee on Food Additives (JECFA) is one of three Codex committees tasked with applying risk analysis and relying on independent scientific advice provided by expert bodies organized by FAO/WHO when developing standards. While not officially part of the Codex Alimentarius Commission structure, JECFA provides independent scientific advice to the Commission and its specialist committees such as the Codex Committee on Residues of Veterinary Drugs in Foods (CCRVDF) in setting maximum residue limits (MRLs) for veterinary drugs. Codex methods of analysis (Types I, II, III, and IV) are defined in the Codex Procedural Manual as are criteria to be used for selecting methods of analysis. However, if a method is to be used under a single laboratory condition to support regulatory work, it must be validated according to an internationally recognized protocol and the use of the method must be embedded in a quality assurance system in compliance with ISO/IEC 17025:2005. This paper examines the attributes of the methods used to generate residue depletion data for drug registration and/or licensing and for supporting regulatory enforcement initiatives that experts consider to be useful and appropriate in their assessment of methods of analysis. Copyright © 2016 Her Majesty the Queen in Right of Canada. Drug Testing and Analysis © 2016 John Wiley & Sons, Ltd.

  5. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF SIMULTANEOUS ESTIMATION OF AMLODIPINE AND ATORVASTATIN BY RP-UPLC

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    Waghmare A. N

    2014-02-01

    Full Text Available Objective: To develop and validate simple, sensitive, robust, rapid and specific isocratic RP-UPLC method for simultaneous estimation of Amlodipine and Atorvastatin in tablet dosage form. Methods: The developed method consisting the mobile phase of acetonitrile and 0.02 M Potassium dihydrogen phosphate (55:45 with isocratic programming, BEH C18 (100mm×2.1mm, 1.7μm column as stationary phase with a flow rate of 0.3 mL/minute. Results and discussion: Proposed method was found to be linear for Amlodipine and Atorvastatin in the concentration range of 0.5 to 40.0 μg/mL with r2 of 0.9999 for Amlodipine and 0.9997 for Atorvastatin respectively. Precision study showed that the percentage relative standard deviation was within the range of acceptable limits, and the mean recovery was found to be 100.79 % for assay of Amlodipine and 99.87% for Atorvastatin in tablet dosage form .The LOD and LOQ of Amlodipine and Atorvastatin were found to be 0.062 and 0.078μg/ml and 0.020 and 0.026 μg/mL.

  6. Development and validation of analytical method for the estimation of lamivudine in rabbit plasma

    Institute of Scientific and Technical Information of China (English)

    Akhilesh Vikram Singh; Lila K. Nath; Nihar R. Pani

    2011-01-01

    Lamivudine has been widely used in the treatment of HIV disease. A reliable, sensitive reversed phase high performance liquid chromatography (RP-HPLC) method was developed and validated for lamivudine in rabbit plasma. The method was developed on Hypersil BDS C-18 column (250 mm * 4.6 mm, 5 μm) using a mobile phase of 0.25% Triethylamine buffer (pH 3.0): acetonitrile (70:30, v/v). The efficient was monitored by UV detector at 256 nm. The total run time was 15 min with a flow rate of 1.0 mL/min. Calibration curve was linear over the concentration range of 25-2000 ng/mL. The retention times of lamivudine and internal standard (Nelfinavir) were 8.78 min and 10.86 min, respectively. The developed RP-HPLC method can be successfully applied for the quantitative pharmacokinetic parameters determination of lamivudine in rabbit model.

  7. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR FLUCONAZOLE AND IVERMECTIN IN TABLET FORMULATION BY USING RP-HPLC

    Directory of Open Access Journals (Sweden)

    Harod S. Sanjay

    2012-08-01

    Full Text Available A simple, efficient and reproducible RP-HPLC method for the simultaneous determination of Fluconazole and Ivermectin in bulk and tablet formulation has been developed and validated. The separation was carried out using Insertil C18 column (250 mm x 4.6 mm, 5 µ using Acetonitrile:Methanol:Water (75:15:10 v/v/v as mobile phase. The flow rate was 1.5 ml/min and detection was carried out 254 nm. The retention time of Fluconazole and Ivermectin were 2.313 and 9.617 respectively. The linear was established in the range of 50-150 µg/ml and 52-156 µg/ml for Fluconazole and Ivermectin respectively. Percentage recoveries for Fluconazole and Ivermectin were found to be 99.830±1.079 and 100.814±1.99 respectively. All the analytical validation parameters were determined and found in the limit as per ICH Guidelines which indicate the validity of the method. The developed method is also found to be precise and robust for the simultaneous determination of Fluconazole and Ivermectin in tablet formulation.

  8. A validated HPLC analytical method for the analysis of solasonine and solamargine in in vitro skin penetration studies

    Directory of Open Access Journals (Sweden)

    Renata F. J. Tiossi

    2012-01-01

    Full Text Available To assess topical delivery studies of glycoalkaloids, an analytical method by HPLC-UV was developed and validated for the determination of solasonine (SN and solamargine (SM in different skin layers, as well as in a topical formulation. The method was linear within the ranges 0.86 to 990.00 µg/mL for SN and 1.74 to 1000.00 µg/mL for SM (r = 0.9996. Moreover, the recoveries for both glycoalkaloids were higher than 88.94 and 93.23% from skin samples and topical formulation, respectively. The method developed is reliable and suitable for topical delivery skin studies and for determining the content of SN and SM in topical formulations.

  9. 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".

    Science.gov (United States)

    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.

  10. [Analytical validation of a chromatographic method dedicated to search and identify natural and semi-synthetic opiates].

    Science.gov (United States)

    Dubois, Nathalie; Counerotte, Stéphane; Goffin, Eric; Pirotte, Bernard; Charlier, Corinne

    2014-01-01

    The identification of a product absorbed by an opiate consumer is sometimes problematic since there is no specific biomarker for all molecules. We developed an ultra-high pressure liquid chromatography coupled to tandem mass spectrometry technique which allows the identification and the quantification of 25 opiates in plasma. The sample preparation consists in a solid-phase extraction on Oasis MCX cartridges (Waters). The method has been validated according to FDA criteria completely for 21 substances and with some reservations for the remaining 4 analytes. This method has been applied to 80 patients treated at the University Hospital of Liege for whom the screening of opiates was positive. The identification of the product consumed was effective in 86% of cases.

  11. Validation of an HPLC analytical method coupled to a multifunctional clean-up column for the determination of deoxynivalenol.

    Science.gov (United States)

    Sugita-Konsihi, Yoshiko; Tanaka, Toshitsugu; Tabata, Setsuko; Nakajima, Masahiro; Nouno, Masanori; Nakaie, Yoko; Chonan, Takao; Aoyagi, Mitsutoshi; Kibune, Nobuyuki; Mizuno, Kazutoshi; Ishikuro, Eiichi; Kanamaru, Naoki; Minamisawa, Masatoshi; Aita, Norio; Kushiro, Masayo; Tanaka, Kenji; Takatori, Kosuke

    2006-04-01

    To evaluate a method using a multifunctional clean-up column coupled with high performance liquid chromatography as an official analytical method for the determination of deoxynivalenol in wheat used as food or feed, an inter-laboratory study was performed in 12 laboratories using four naturally contaminated wheat samples and one spiked sample. The relative standard deviations for repeatability (RSDr) and reproducibility (RSDR) of naturally contaminated wheat were in the range 5.8-11.3% and 12.0-20.7%, respectively. The HORRAT was less than 1.0 in each sample. From the spiking test, the recovery rate, RSDr, RSDR and HORRAT value were 100.0%, 11.2%, 10.3% and 0.5, respectively. The limit of quantification is 0.10 mg/kg from the range obtained in a linear calibration. Thus, it should be useful as a sensitive and validated analytical method for the determination of deoxynivalenol in wheat intended for use in food and feed.

  12. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF METAXALONE IN BULK AND ITS PHARMACEUTICAL FORMULATION BY UV SPECTROSCOPIC METHOD

    Directory of Open Access Journals (Sweden)

    N. V. Mahipal Reddy

    2013-03-01

    Full Text Available Metaxalone, a muscle relaxant used to relax muscles and relieve pain caused by strains, sprains and othermusculoskeletal conditions. A simple, accurate, precise, reproducible, highly sensitive, economic UV spectrophotometric method has been developed for the estimation of metaxalon in bulk and tablet dosage form. In this method metaxalon showed maximum absorbance at 280 nm in methanol. The developed spectrophotometric method was validated in accordance with ICH guidelines. Linearity of the method was found to be 5 - 160µg/ml. The method obeyed Beer’s law in the concentration range of 5 -160 µg/ml. The LOD and LOQ were found to be 3.489μg/ml and 10.575μg/ml respectively. A mean recovery of metaxalon in tablet dosage form was found to be 99.69%.the method was found to be simple, accurate, precise, specific, sensitive, reproducible and can be directly and easily applied to tablet dosage form.

  13. Development and validation of new analytical method for acrolein in air.

    Science.gov (United States)

    Yasuhara, A; Dennis, K J; Shibamoto, T

    1989-01-01

    A new method was developed to determine vapor-phase acrolein in air samples. Air containing vapor-phase acrolein was purged into impingers filled with a dichloromethane solution of N-methylhydrazine. The resulting derivative, 1-methyl-2-pyrazoline, was analyzed by gas chromatography using a nitrogen-phosphorous detector (NPD). The detection limit was 8.9 pg 1-methyl-2-pyrazoline, equivalent to 5.9 pg acrolein. The recovery efficiencies of vapor-phase acrolein were 98.0 +/- 2.9% and 100.3 +/- 3.1% for 150 and 15 micrograms, respectively. This method was satisfactorily applied for determination of acrolein formed from various heated fats. The amounts of acrolein formed in a headspace were 109 micrograms/L from lard, 164 micrograms/L from corn oil, 5.1 micrograms/L from cotton seed oil, and 163 micrograms/L from sunflower oil.

  14. Quantification of urinary chorionic gonadotropin in spontaneous abortion of pre-clinically recognized pregnancy: method development and analytical validation.

    Science.gov (United States)

    Reis, M Fátima; Aniceto, Pedro; Aguiar, Pedro; Simão, Filipa; Segurado, Susana

    2007-05-01

    Determination of environmental impacts on reproductive health and specifically on the incidence of early spontaneous abortion requires accurate estimates of the latter. This negative reproductive outcome can be detected by the pattern of elevation and decline of human chorionic gonadotropin (hCG) levels near and shortly beyond the expected time of implantation, requiring daily biomonitoring of hCG levels during the relevant period of the menstrual cycle. Prospective pregnancy studies to assess effects of potentially toxic exposures on human reproductive outcomes can involve up to three menstrual cycles and a huge number of samples in each, for the quantification of the inherently very low hCG levels usually can be determined only in serum. The invasive nature of blood collection, the number of samples needed for the development of prospective studies, and the lack of quantitative methods for the determination of low hCG levels in urine point to the need for collecting urine rather than blood and make it imperative to develop suitable quantitative methods for biomonitoring of very low levels of hCG in urine. This paper describes the development and validation procedures of an automated solid-phase two-site chemiluminescent immunometric assay for the quantification of urinary hCG in early pregnancy and early pregnancy loss. For the validation, both undiluted and diluted urine and control samples have been prepared. From the results, it can be concluded that the assay has a calibration range that extends to 5000 mIU/ml, with a detection limit of approximately 1.2 mIU/ml, practically identical to that found by the IMMULITE 2000 manufacturer's validation study. The intra- and inter-assay precision ranges up to a maximum of around 7%, meaning that the practical limit for functional sensitivity can be established as low as 10%. This means that the immunoassay from DPC can identify, with relatively high confidence, non-pregnant women and the typical "rise and fall" pattern

  15. Development and validation of a stability-indicating analytical method for the quantitation of oxytocin in pharmaceutical dosage forms.

    Science.gov (United States)

    Chaibva, F A; Walker, R B

    2007-01-04

    A single stability-indicating assay for oxytocin (OT) in pharmaceutical dosage forms using gradient elution over 21 min has been reported in the literature. Furthermore, published and compendial methods for the analysis of OT containing dosage forms also involve using HPLC with gradient elution and complicated mobile phases that include hydrophobic ion pairing agents. A simple isocratic and stability-indicating assay was developed and validated. The conditions are as follows, column: Phenomenex C18 Hypersil, 5 microm packing, 4.6 mm x 150 mm with acetonitrile-phosphate buffer (pH 5; 0.08 M) (20:80) as the mobile phase with UV detection at 220 nm The method was found to be specific for OT in the presence of degradation products and chlorbutol (preservative) with an overall analytical run time of 16 min. Accuracy was determined to be 0.77-1.18% bias for all samples tested. Intra-assay precision (repeatability) was found to be 0.22-1.04%R.S.D. while the inter-day precision (intermediate precision) was found to be 1.27-1.68%R.S.D. for the samples studied. The calibration curve was found to be linear with the equation y = 1.81x + 0.02 and a linear regression coefficient of 0.9991 over the range 0.4-12.0 IU/ml. The LOD and the LOQ were determined to be 0.1 and 0.4 IU/ml, respectively. Syntocinon, a commercially available dosage form of OT was assayed resulting in 100.5-106.6% recovery of the label claim and an average of 10.04 IU/ml.

  16. Validation of an analytical method for the determination of spiramycin, virginiamycin and tylosin in feeding-stuffs bij thin-layer chromatography and bio-autography

    NARCIS (Netherlands)

    Vincent, U.; Gizzi, G.; Holst, von C.; Jong, de J.; Michard, J.

    2007-01-01

    An inter-laboratory validation was carried out to determine the performance characteristics of an analytical method based on thin-layer chromatography (TLC) coupled to microbiological detection (bio-autography) for screening feed samples for the presence of spiramycin, tylosin and virginiamycin. Twe

  17. Validation of selected analytical methods using accuracy profiles to assess the impact of a Tobacco Heating System on indoor air quality.

    Science.gov (United States)

    Mottier, Nicolas; Tharin, Manuel; Cluse, Camille; Crudo, Jean-René; Lueso, María Gómez; Goujon-Ginglinger, Catherine G; Jaquier, Anne; Mitova, Maya I; Rouget, Emmanuel G R; Schaller, Mathieu; Solioz, Jennifer

    2016-09-01

    Studies in environmentally controlled rooms have been used over the years to assess the impact of environmental tobacco smoke on indoor air quality. As new tobacco products are developed, it is important to determine their impact on air quality when used indoors. Before such an assessment can take place it is essential that the analytical methods used to assess indoor air quality are validated and shown to be fit for their intended purpose. Consequently, for this assessment, an environmentally controlled room was built and seven analytical methods, representing eighteen analytes, were validated. The validations were carried out with smoking machines using a matrix-based approach applying the accuracy profile procedure. The performances of the methods were compared for all three matrices under investigation: background air samples, the environmental aerosol of Tobacco Heating System THS 2.2, a heat-not-burn tobacco product developed by Philip Morris International, and the environmental tobacco smoke of a cigarette. The environmental aerosol generated by the THS 2.2 device did not have any appreciable impact on the performances of the methods. The comparison between the background and THS 2.2 environmental aerosol samples generated by smoking machines showed that only five compounds were higher when THS 2.2 was used in the environmentally controlled room. Regarding environmental tobacco smoke from cigarettes, the yields of all analytes were clearly above those obtained with the other two air sample types.

  18. Validation of a UV-spectrophotometric analytical method for determination of LPSF/AC04 from inclusion complex and liposomes

    Directory of Open Access Journals (Sweden)

    Rafaela Siqueira Ferraz

    2015-03-01

    Full Text Available The aim of this study was to develop and validate a UV spectrophotometric method for determination of LPSF/AC04 from inclusion complex and encapsulated into liposomes. The validation parameters were determined according to the International Conference on Harmonisation (ICH and National Health Surveillance Agency (ANVISA guidelines. LPSF/AC04 was determined at 250 nm in methanol by a UV spectrophotometric method, exhibiting linearity in the range from 0.3 to 2 µg.mL−1 (Absorbance=0.18068 x [LPSF/AC04 µg.mL-1] + 0.00348, (r2=0.9995. The limits of detection and quantification were 0.047µg.mL−1 and 0.143µg.mL−1, respectively. The method was accurate, precise, reproducible and robust since all the samples analyzed had coefficient of variation of less than 5% and no statistically significant difference between theoretical and practical concentrations was detected. Thus, a rapid, simple, low cost and sensitive spectrophotometric method was developed and validated for determining the content of inclusion complex and liposomes containing LPSF/AC04.

  19. Analytical Method Development and Validation of Esomeprazole and Levosulpiride in their Combined Capsule Dosage Form by RP-HPLC

    Directory of Open Access Journals (Sweden)

    Patel H

    2012-07-01

    Full Text Available A new simple, accurate, rapid and precise isocratic Reverse Phase High performance liquid chromatographic (HPLC method was developed and validated for the determination of Esomeprazole (ESO, and Levosulpiride (LEVO in capsule formulation. The Method employs Shimadzu HPLC system on Hypercil BDS C18 (25 cm × 4.6 mm i.e., 5 µm and flow rate of 1 ml/min with a load of 20µl. Acetonitrile and Phosphate buffer was used as mobile phase in the composition of 50:50 at 3.5 PH. The Detection was carried out at 240 nm. Linearity ranges for Esomeprazole and Levosulpiride were 20-60 µg/ml, 37.5-225 µg/ml respectively. Retention Time of Levosulpiride and Esomeprazole were found to be 3.367 min, 4.320 min respectively. Percent Recovery study values of Esomeprazole and Levosulpiride were found to be within 98-102%. This newly developed method was successfully utilized for the Quantitative estimation of Esomeprazole and Levosulpiride in pharmaceutical dosage forms. This method was validated for accuracy, precision, linearity and Robustness as per ICH guidelines.

  20. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR FLUCONAZOLE AND IVERMECTIN IN TABLET FORMULATION BY USING RP-HPLC

    OpenAIRE

    Harod S. Sanjay; Manocha Nimita; Hingole Ashwin; Dubey P.K.

    2012-01-01

    A simple, efficient and reproducible RP-HPLC method for the simultaneous determination of Fluconazole and Ivermectin in bulk and tablet formulation has been developed and validated. The separation was carried out using Insertil C18 column (250 mm x 4.6 mm, 5 µ) using Acetonitrile:Methanol:Water (75:15:10 v/v/v) as mobile phase. The flow rate was 1.5 ml/min and detection was carried out 254 nm. The retention time of Fluconazole and Ivermectin were 2.313 and 9.617 respectively. The linear was e...

  1. Bio-analytical method development and validation of Rasagiline by high performance liquid chromatography tandem mass spectrometry detection and its application to pharmacokinetic study

    Institute of Scientific and Technical Information of China (English)

    Ravi Kumar Konda; Babu Rao Chandu; B.R. Challa; Chandrasekhar B. Kothapalli

    2012-01-01

    The most suitable bio-analytical method based on liquid liquid extraction has been developed and validated for quantification of Rasagiline in human plasma. Rasagiline-13C3 mesylate was used as an internal standard for Rasagiline. Zorbax Eclipse Plus C18 (2.1 mm × 50 mm, 3.5 um) column provided chromatographic separation of analyte followed by detection with mass spectrometry. The method involved simple isocratic chromatographic condition and mass spectrometric detection in the positive ionization mode using an API-4000 system. The lotal run time was 3.0 min. The proposed method has been validated with the linear range of 5 12000 pg/mL for Rasagiline. The intra-run and inter-run precision values were within 1.3% 2.9% and 1.6% 2.2% respectively for Rasagiline. The overall recovery for Rasagiline and Rasagiline-13C3 mesylate analog was 96.9% and 96.7% respectively. This validated method was successfully applied to the bioequivalence and pharmacokinetic study of human volunteers under fasting condition.

  2. Determination of ochratoxin A in liquorice products using HPLC-based analytical methods. Part II: harmonised method and method validation study.

    Science.gov (United States)

    Raters, Marion; Matissek, Reinhard; van Haren, Winni; Fledderus, Koop

    2010-05-01

    On the basis of the outcome of an European proficiency test series conducted on behalf of the CAOBISCO (Association of the Chocolate, Biscuit and Confectionery Industries of the EU) expert group on ochratoxin A, a new harmonised method was developed for the analysis of ochratoxin A in liquorice extracts. This method works without the use of halogenated solvents because, as the proficiency test showed, an aqueous extraction solution can be used instead of, for example, chloroform, whose use is restricted in the EU. The main objective of this method validation study was to check the performance of this harmonised method. To carry out the method validation study, a set of three different test samples (one liquorice powder and two liquorice pastes) and a liquorice powder sample with an indicated range of ochratoxin A (a so-called sunshine sample) was distributed to 21 laboratories in ten countries throughout Europe and to one laboratory in the USA. The study was evaluated according to internationally recognised guidelines. In terms of its repeatability and reproducibility for determining ochratoxin A in liquorice extracts with a relative standard deviation for repeatability (RSDr) of between 6.68 and 19.95 and a relative standard deviation for reproducibility (RSDR) of between 17.39 and 29.08 the performance of the harmonised method was found to be in the accepted range of the EU directive for the analysis of mycotoxins in several foodstuffs.

  3. Occupational exposure to polycyclic aromatic hydrocarbons in airborne particulate matter: validation and application of a gas chromatography-mass spectrometry analytical method.

    Science.gov (United States)

    Fioretti, Marzia; Catrambone, Tamara; Gordiani, Andrea; Cabella, Renato

    2010-12-01

    This study concerns the validation of an analytical method for the measurement of occupational exposure to trace levels of polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matter (APM). Personal exposure to selected PAHs of five workers occupationally exposed to urban pollution in Rome, Italy, was evaluated. The samples were collected over 10 days evenly distributed during winter and summer of 2008. Polycyclic aromatic hydrocarbons were collected by a sampling pump and trapped in polytetrafluoroethylene filters; ultrasonic extraction was applied to extract PAH species from the matrix with toluene, and the concentrated extract was quantitatively analyzed by GC/MS. The analytical method was optimized and validated using a standard reference material of urban dust (SRM 1649a). Detection limits ranged from 0.8 ng per sample for indeno [1,2,3-cd] pyrene to 20.4 ng for sample for anthracene. Experimental results of the 50 personal samples collected showed that phenanthrene was the predominant polycyclic aromatic hydrocarbon [95% CI (32.42-41.13 ng m(-3))]; the highest benzo[a]pyrene concentration was 2.58 ng m(-3), approximately 2-fold higher than European annual target values (1 ng m(-3)). Seasonal variations of personal exposure to selected PAHs suggested higher emissions and reduced atmospheric reactivity of PAH compounds in winter. The analytical method was a suitable procedure for the determination of 13 of the 16 priority PAHs in APM personal samples and can be considered a useful tool to evaluate occupational exposure to low PAH levels.

  4. HPLC法验证中有关问题探讨%Elaboration on the Validation of HPLC Analytical Method

    Institute of Scientific and Technical Information of China (English)

    夏振华; 王颖异; 王赞朋

    2016-01-01

    方法验证虽然有包括《中国药典》在内的许多指南,但《指南》一般较为原则性,没有具体操作指导,如有关物质测定方法的线性范围如何确定?耐用性进行哪些项目较为科学?验证项目是否都需要加入样品以考察干扰?精密度误差接受标准是什么?这些都是在实际验证中非常纠结的问题,而且《指南》也未必所有内容都科学,诸如强降解试验的物料平衡问题、峰纯度测定问题等,笔者结合近30年的工作经验,对HPLC分析方法验证的实际操作的疑点和难点进行探讨。%While there are many guidelines about method validation, like those in the Chinese Pharmacopoeia, guidelines generally include general principles without specific operations. Many problems are very tangled in practice, such as how to determine the linear range of related substance; what is the more scientific variables to be chosen in durability tests; is it necessary to examine interference by adding samples in each methodology validation project; how to determine acceptance criteria of intermediate precision, etc. And not all the guidelines are scientific, such as mass balance and peak purity in stress tests, etc. The authors, combining years of experiences, analyze the doubts and difficulties in actual operation of HPLC analysis method validation.

  5. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF SOLID DOSAGE FORM OF ANTINEOPLASTIC DRUG IMATINIB MESILATE BY RP HPLC.

    Directory of Open Access Journals (Sweden)

    G. Sathwik

    2015-04-01

    Full Text Available A simple and sensitive High Performance Liquid Chromatographic method has been established and validated for Imatinib Mesylate in pharmaceutical dosage form, separation was performed on a C18, 150×4.6 mm, 5μ column in isocratic mode, with mobile phase containing a mixture of buffer: acetonitrile (72:28 v/v. The mobile phase was pumped at a flow rate of 1.0 ml/min and eluents were monitored at 265 nm. Linearity was found to be in the range of levels 80% to 120% and retention time was 3.63 min. The statistical validation parameters such as linearity, accuracy, precision, and specificity, limit of detection, limit of quantification were checked. The samples were prepared in water and the stability of Imatinib mesylate in aqueous solution at 30°C was studied. The results were satisfactory with good stability after 24 h at 30°C. The proposed method can be used for the related substances of Imatinib mesylate.

  6. An evaluation of 25B-, 25C-, 25D-, 25H-, 25I- and 25T2-NBOMe via LC-MS-MS: method validation and analyte stability.

    Science.gov (United States)

    Johnson, Robert D; Botch-Jones, Sabra R; Flowers, Tiffany; Lewis, Connie A

    2014-10-01

    As potent serotonin (5-HT2A) receptor agonists, the NBOMe class of drugs including 25B-, 25C-, 25D-, 25H-, 25I- and 25T2-NBOMe is frequently abused due to the intense hallucinations that they induce. From the limited literature available, the concentration of these NBOMe compounds reported in postmortem cases is exceedingly low. In most instances, published concentrations are NBOMe, evaluation of 25B-, 25C-, 25D-, 25H and 25T2- in whole blood, plasma and urine was conducted. This publication presents the data obtained from the validation of a liquid chromatography-tandem mass spectrometry method for the simultaneous quantification of these six NBOMe analogs. The method utilizes ultra-performance liquid chromatography technology for the separation followed by positive electrospray ionization of each analog. Limits of quantification for these analogs ranged from 0.01 to 0.02 ng/mL (10-20 pg/mL) with typical linear dynamic ranges of 0.01-20 ng/mL. Data for recovery, intraday control accuracy and precision, matrix effects, ion suppression/enhancement and analyte stability are included. Validation was completed in whole blood, plasma and urine. Short run times and high sensitivity afforded by this newly validated analytical method that allows for the detection of these six analogs in the most common toxicological matrices and can be applied to both ante- and postmortem specimens.

  7. Validation of an analytical method for simultaneous high-precision measurements of greenhouse gas emissions from wastewater treatment plants using a gas chromatography-barrier discharge detector system.

    Science.gov (United States)

    Pascale, Raffaella; Caivano, Marianna; Buchicchio, Alessandro; Mancini, Ignazio M; Bianco, Giuliana; Caniani, Donatella

    2017-01-13

    Wastewater treatment plants (WWTPs) emit CO2 and N2O, which may lead to climate change and global warming. Over the last few years, awareness of greenhouse gas (GHG) emissions from WWTPs has increased. Moreover, the development of valid, reliable, and high-throughput analytical methods for simultaneous gas analysis is an essential requirement for environmental applications. In the present study, an analytical method based on a gas chromatograph (GC) equipped with a barrier ionization discharge (BID) detector was developed for the first time. This new method simultaneously analyses CO2 and N2O and has a precision, measured in terms of relative standard of variation RSD%, equal to or less than 6.6% and 5.1%, respectively. The method's detection limits are 5.3ppmv for CO2 and 62.0ppbv for N2O. The method's selectivity, linearity, accuracy, repeatability, intermediate precision, limit of detection and limit of quantification were good at trace concentration levels. After validation, the method was applied to a real case of N2O and CO2 emissions from a WWTP, confirming its suitability as a standard procedure for simultaneous GHG analysis in environmental samples containing CO2 levels less than 12,000mg/L.

  8. Development and validation of an analytical method for the quantification of cytochrome c in skin transport studies.

    Science.gov (United States)

    Bachhav, Yogeshwar G; Kalia, Yogeshvar N

    2010-07-01

    A simple isocratic HPLC method for the quantification of Cytochrome c in skin permeation samples was developed and validated. The mobile phase comprised a 41 : 59 mixture of an organic phase A (0.1% trifluoroacetic acid in a 90 : 10 mixture of MeCN-H(2)O) and an aqueous phase B (0.1% trifluoroacetic acid in H(2)O). The Cytochrome c retention and run times were 2.62 and 8.0 min, respectively--much shorter than those for existing gradient methods. The response was accurate, precise and linear from 2.5 to 25 microg/mL. The mean recoveries for intra-day and inter-day analysis ranged from 88.5 to 103.8% and the RSD varied from 0.05 to 1.55%. The assay was used to quantify transport of Cytochrome c across intact and laser-microporated porcine skin in vitro. Cytochrome c permeation and the amount of protein retained within the membrane over 24 h were quantified as a function of the number of micropores. Although no Cytochrome c permeation was observed across intact skin, laser microporation enabled delivery of 22.9 +/- 3.3 and 56.0 +/- 15.9 microg/cm(2) of the protein across skin samples with 300 and 1800 micropores, respectively. In conclusion, the HPLC method provided a fast, efficient means to quantify Cytochrome c in samples from skin transport studies.

  9. Development and validation of an analytical method for the extraction and quantification of soluble sulfates in red clay

    Directory of Open Access Journals (Sweden)

    V. I. Cáceres

    2015-09-01

    Full Text Available AbstractIn this work a fast and environmentally friendly method for the extraction and quantification of soluble sulphates in red clay using microwave assisted extraction (MAE and determination by turbidimetry was developed and validated. The favorable conditions for the extraction of soluble sulphates in red clay by MAE were: 1 g of sample, with particle size of 63μm, dissolved in 50 mL of distilled water, it was extracted using a microwave oven with 70% of power during 5 min, later the sample was centrifuged during 5 min and then filtered. The soluble sulphates in red clays were quantified at 420 nm. The procedure proposed showed linear behaviour in the tested rank (5-7000 mg SO42-/kg of clay with R2 0.9993. The limits of detection and quantification were 4.30 and 14.33 mg/kg, respectively, with a variation coefficient of 1.41%. The method proposed in this work allows to determine soluble sulphates in red clay with a recovery of 94%.

  10. Dried blood spot specimen quality and validation of a new pre-analytical processing method for qualitative HIV-1 PCR, KwaZulu-Natal, South Africa

    Directory of Open Access Journals (Sweden)

    Kerusha Govender

    2016-02-01

    Full Text Available Background: Poor quality dried blood spot (DBS specimens are usually rejected by virology laboratories, affecting early infant diagnosis of HIV. The practice of combining two incompletely-filled DBS in one specimen preparation tube during pre-analytical specimen processing (i.e., the two-spot method has been implemented to reduce the number of specimens being rejected for insufficient volume.Objectives: This study analysed laboratory data to describe the quality of DBS specimens and the use of the two-spot method over a one-year period, then validated the two-spot method against the standard (one-spot method.Methods: Data on HIV-1 PCR test requests submitted in 2014 to the Department of Virology at Inkosi Albert Luthuli Central Hospital in KwaZulu-Natal province, South Africa were analysed to describe reasons for specimen rejection, as well as results of the two-spot method. The accuracy, lower limit of detection and precision of the two-spot method were assessed.Results: Of the 88 481 specimens received, 3.7% were rejected for pre-analytical problems. Of those, 48.9% were rejected as a result of insufficient specimen volume. Two health facilities had significantly more specimen rejections than other facilities. The two-spot method prevented 10 504 specimen rejections. The Pearson correlation coefficient comparing the standard to the two-spot method was 0.997.Conclusions: The two-spot method was comparable with the standard method of pre-analytical specimen processing. Two health facilities were identified for targeted retraining on specimen quality. The two-spot method of DBS specimen processing can be used as an adjunct to retraining, to reduce the number of specimens rejected and improve linkage to care.

  11. Validation of analytical methods in GMP: the disposable Fast Read 102® device, an alternative practical approach for cell counting

    Directory of Open Access Journals (Sweden)

    Gunetti Monica

    2012-05-01

    Full Text Available Abstract Background The quality and safety of advanced therapy products must be maintained throughout their production and quality control cycle to ensure their final use in patients. We validated the cell count method according to the International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use and European Pharmacopoeia, considering the tests’ accuracy, precision, repeatability, linearity and range. Methods As the cell count is a potency test, we checked accuracy, precision, and linearity, according to ICH Q2. Briefly our experimental approach was first to evaluate the accuracy of Fast Read 102® compared to the Bürker chamber. Once the accuracy of the alternative method was demonstrated, we checked the precision and linearity test only using Fast Read 102®. The data were statistically analyzed by average, standard deviation and coefficient of variation percentages inter and intra operator. Results All the tests performed met the established acceptance criteria of a coefficient of variation of less than ten percent. For the cell count, the precision reached by each operator had a coefficient of variation of less than ten percent (total cells and under five percent (viable cells. The best range of dilution, to obtain a slope line value very similar to 1, was between 1:8 and 1:128. Conclusions Our data demonstrated that the Fast Read 102® count method is accurate, precise and ensures the linearity of the results obtained in a range of cell dilution. Under our standard method procedures, this assay may thus be considered a good quality control method for the cell count as a batch release quality control test. Moreover, the Fast Read 102® chamber is a plastic, disposable device that allows a number of samples to be counted in the same chamber. Last but not least, it overcomes the problem of chamber washing after use and so allows a cell count in a clean environment such as that in a

  12. Sewage-based epidemiology in monitoring the use of new psychoactive substances: Validation and application of an analytical method using LC-MS/MS.

    Science.gov (United States)

    Kinyua, Juliet; Covaci, Adrian; Maho, Walid; McCall, Ann-Kathrin; Neels, Hugo; van Nuijs, Alexander L N

    2015-09-01

    Sewage-based epidemiology (SBE) employs the analysis of sewage to detect and quantify drug use within a community. While SBE has been applied repeatedly for the estimation of classical illicit drugs, only few studies investigated new psychoactive substances (NPS). These compounds mimic effects of illicit drugs by introducing slight modifications to chemical structures of controlled illicit drugs. We describe the optimization, validation, and application of an analytical method using liquid chromatography coupled to positive electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of seven NPS in sewage: methoxetamine (MXE), butylone, ethylone, methylone, methiopropamine (MPA), 4-methoxymethamphetamine (PMMA), and 4-methoxyamphetamine (PMA). Sample preparation was performed using solid-phase extraction (SPE) with Oasis MCX cartridges. The LC separation was done with a HILIC (150 x 3 mm, 5 µm) column which ensured good resolution of the analytes with a total run time of 19 min. The lower limit of quantification (LLOQ) was between 0.5 and 5 ng/L for all compounds. The method was validated by evaluating the following parameters: sensitivity, selectivity, linearity, accuracy, precision, recoveries and matrix effects. The method was applied on sewage samples collected from sewage treatment plants in Belgium and Switzerland in which all investigated compounds were detected, except MPA and PMA. Furthermore, a consistent presence of MXE has been observed in most of the sewage samples at levels higher than LLOQ.

  13. Analytical method (HPLC, validation used for identification and assay of the pharmaceutical active ingredient, Tylosin tartrate for veterinary use and its finite product Tilodem 50, hydrosoluble powder

    Directory of Open Access Journals (Sweden)

    Maria Neagu

    2010-12-01

    Full Text Available In SC DELOS IMPEX ’96 SRL the quality of the active pharmaceutical ingredient (API for the finite product Tilodem 50 - hydrosoluble powder was acomkplished in the respect of last European Pharmacopoeia.The method for analysis used in this purpose was the compendial method „Tylosin tartrate for veterinary use” in EurPh. in vigour edition and represent a variant developed and validation „in house”.The parameters which was included in the methodology validation for chromatographic method are the followings: Selectivity, Linearity, Linearity range, Detection and Quantification limits, Precision, Repeatability (intra day, Inter-Day Reproductibility, Accuracy, Robustness, Solutions’ stability and System suitability. According to the European Pharmacopoeia, the active pharmaceutical ingredient is consistent, in terms of quality, if it contains Tylosin A - minimum 80% and the amount of Tylosin A, B, C, D, at minimum 95%. Identification and determination of each component separately (Tylosin A, B, C, D is possible by chromatographic separation-HPLC. Validation of analytical methods is presented below.

  14. Development and analytical validation of a screening method for simultaneous detection of five adulterants in raw milk using mid-infrared spectroscopy and PLS-DA.

    Science.gov (United States)

    Botelho, Bruno G; Reis, Nádia; Oliveira, Leandro S; Sena, Marcelo M

    2015-08-15

    This paper proposed a new screening method for the simultaneous detection of five common adulterants in raw cow milk by using attenuated total reflectance (ATR) mid infrared spectroscopy and multivariate supervised classification (partial least squares discrimination analysis - PLSDA). The method was able to detect the presence of the adulterants water, starch, sodium citrate, formaldehyde and sucrose in milk samples containing from one up to five of these analytes, in the range of 0.5-10% w/v. A multivariate qualitative validation was performed, estimating specific figures of merit, such as false positive and false negative rates, selectivity, specificity and efficiency rates, accordance and concordance. The proposed method does not need any sample pretreatment, requires a small amount of sample (30 μL), is fast and simple, being suitable for the control of raw milk in a dairy industry or for the quality inspection of commercialized milk.

  15. Development and validation of an HPLC-MS/MS method to quantify clopidogrel acyl glucuronide, clopidogrel acid metabolite, and clopidogrel in plasma samples avoiding analyte back-conversion.

    Science.gov (United States)

    Silvestro, Luigi; Gheorghe, Mihaela; Iordachescu, Adriana; Ciuca, Valentin; Tudoroniu, Ariana; Rizea Savu, Simona; Tarcomnicu, Isabela

    2011-08-01

    A new sensitive and fast quantitative analytical method for the simultaneous determination of clopidogrel, its main metabolite clopidogrel carboxylic acid, and the newly described acyl glucuronide metabolite, in human plasma samples, is presented. The analytical procedures (plasma storage, handling, and extract storage in the autosampler) were optimized in order to avoid back-conversion; a known drawback in measurements of clopidogrel. Clopidogrel acyl glucuronide was confirmed as a major source of back-conversion to the parent drug in the presence of methanol, and thorough stability experiments were carried out to find the most appropriate conditions for an accurate analysis of clopidogrel and the two metabolites. The method was validated by assessing selectivity, sensitivity, linearity, accuracy, and precision for all three analytes, in accordance to Food and Drug Administration guidelines. Spiked quality controls in plasma as well as incurred samples were used to verify back-conversion in the selected conditions, with results meeting European Medicines Agency acceptance criteria (concentrations within 80-120% of the first reading). The method was then applied to a pharmacokinetic study, and for the first time, a pharmacokinetic curve of clopidogrel acyl glucuronide in human plasma is presented. The concentrations ranged up to 1,048.684 ng/mL, with a mean of 470.268 ng/mL, while clopidogrel had a mean C(max) of 1.348 ng/mL; these orders of magnitude show how much the back-conversion of this metabolite may influence clopidogrel quantification if it is not properly controlled.

  16. Validation of an analytical method for the determination of spiramycin, virginiamycin and tylosin in feeding-stuffs by thin-layer chromatography and bio-autography.

    Science.gov (United States)

    Vincent, Ursula; Gizzi, Gisele; von Holst, Christoph; De Jong, Jacob; Michard, Jacques

    2007-04-01

    An inter-laboratory validation was carried out to determine the performance characteristics of an analytical method based on thin-layer chromatography (TLC) coupled to microbiological detection (bio-autography) for screening feed samples for the presence of spiramycin, tylosin and virginiamycin. Twenty-four samples including blank samples and samples with concentrations of the target analytes ranging between 1 and 5 mg kg(-1) (expressed in microbiological activity) were analysed by seven laboratories participating in the study. The required detection limit was 1 mg kg(-1) (expressed in microbiological activity). For spiramycin, acceptable values for the sensitivity (at least 95%) indicating the rate of correct positive results were obtained for samples containing this substance at or above 2 mg kg(-1), whereas at 1 mg kg(-1), the sensitivity rate dropped to about 70%. Therefore, it was concluded that the detection limit was 2 mg kg(-1). For tylosin and virginiamycin, acceptable values of the sensitivity were obtained for all concentrations including 1 mg kg(-1). Therefore, the method fulfils the criterion regarding the required sensitivity at the target detection limit for tylosin and virginiamycin.

  17. Development, validation and application of a sensitive analytical method for residue determination and dissipation of imidacloprid in sugarcane under tropical field condition.

    Science.gov (United States)

    Ramasubramanian, T; Paramasivam, M; Nirmala, R

    2016-06-01

    A simple and sensitive analytical method has been developed and validated for the determination of trace amounts of imidacloprid in/on sugarcane sett, stalk and leaf. The method optimized in the present study requires less volume of organic solvent and time. Hence, this method is suitable for high-throughput analyses involving large number of samples. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 0.003 and 0.01 mg/kg, respectively. The recovery and relative standard deviation were more than 93 % and less than 4 %, respectively. Thus, it is obvious that the analytical method standardized in this study is more precise and accurate enough to determine the residues of imidacloprid in sugarcane sett, stalk and leaf. The dissipation and translocation of imidacloprid residues from treated cane setts to leaf and stalk were studied by adopting this method. In sugarcane setts, the residues of imidacloprid persisted up to 120 days with half-life of 15.4 days at its recommended dose (70 g a.i./ha). The residues of imidacloprid were found to be translocated from setts to stalk and leaf. The imidacloprid residues were detected up to 105 days in both leaf and stalk. Dipping of sugarcane setts in imidacloprid at its recommended dose may result in better protection of cane setts and established crop because of higher initial deposit (>100 mg/kg) and longer persistence (>120 days).

  18. Systematic Development and Validation of a Thin-Layer Densitometric Bioanalytical Method for Estimation of Mangiferin Employing Analytical Quality by Design (AQbD) Approach.

    Science.gov (United States)

    Khurana, Rajneet Kaur; Rao, Satish; Beg, Sarwar; Katare, O P; Singh, Bhupinder

    2016-01-01

    The present work aims at the systematic development of a simple, rapid and highly sensitive densitometry-based thin-layer chromatographic method for the quantification of mangiferin in bioanalytical samples. Initially, the quality target method profile was defined and critical analytical attributes (CAAs) earmarked, namely, retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Face-centered cubic design was selected for optimization of volume loaded and plate dimensions as the critical method parameters selected from screening studies employing D-optimal and Plackett-Burman design studies, followed by evaluating their effect on the CAAs. The mobile phase containing a mixture of ethyl acetate : acetic acid : formic acid : water in a 7 : 1 : 1 : 1 (v/v/v/v) ratio was finally selected as the optimized solvent for apt chromatographic separation of mangiferin at 262 nm withRf 0.68 ± 0.02 and all other parameters within the acceptance limits. Method validation studies revealed high linearity in the concentration range of 50-800 ng/band for mangiferin. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity and recovery. In a nutshell, the bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin.

  19. Development and validation of a 48-target analytical method for high-throughput monitoring of genetically modified organisms.

    Science.gov (United States)

    Li, Xiaofei; Wu, Yuhua; Li, Jun; Li, Yunjing; Long, Likun; Li, Feiwu; Wu, Gang

    2015-01-05

    The rapid increase in the number of genetically modified (GM) varieties has led to a demand for high-throughput methods to detect genetically modified organisms (GMOs). We describe a new dynamic array-based high throughput method to simultaneously detect 48 targets in 48 samples on a Fludigm system. The test targets included species-specific genes, common screening elements, most of the Chinese-approved GM events, and several unapproved events. The 48 TaqMan assays successfully amplified products from both single-event samples and complex samples with a GMO DNA amount of 0.05 ng, and displayed high specificity. To improve the sensitivity of detection, a preamplification step for 48 pooled targets was added to enrich the amount of template before performing dynamic chip assays. This dynamic chip-based method allowed the synchronous high-throughput detection of multiple targets in multiple samples. Thus, it represents an efficient, qualitative method for GMO multi-detection.

  20. Analytical method development and validation of Drotaverine Hydrochloride and Aceclofenac in bulk and pharmaceutical dosage forms by UV-Spectrophotometer

    OpenAIRE

    Ram Babu Durgam; Sireesha. D; V. V. L. N Prasad; Diwan, Prakash V.

    2013-01-01

    New simple, precise, rapid and reproducible UV-spectrophotometric method has been developed for the estimation of Drotaverine Hydrochloride and Aceclofenac in both bulk and tablet formulation. Drotaverine and Aceclofenac in combined tablet formulation were estimated by using the multicomponent mode at 307 nm for Drotaverine and 276 nm for Aceclofenac in their solution in ethanol: distilled water in the ratio of 50:50 (v/v %), With correlation coefficient of 0.999 for the both the drugs. The B...

  1. Chromatographic development of validated analytical method for the estimation of tapentadol and paracetamol in combined dosage form

    Directory of Open Access Journals (Sweden)

    Manoj S. Charde

    2014-01-01

    Full Text Available A simple, sensitive an isocratic RP-HPLC method for the estimation of  TAP (Tapentadol and PARA (Paracetamol in combined dosage form using Inertsil ODS C-18 column (250×4.6 mm, 5 µ in an isocratic mode with mobile phase comprising  Buffer (1mL TEA :  ACN : MeOH in the ratio of (75:20:5 v/v/v. The flow rate was 1.2 mL/ min and effluent was monitored at 220 nm. The retention times were found to be 6.88 min for TAP and 3.78 min for PARA. The assay exhibited a linear dynamic range of 11.89- 28.55 µg/mL for TAP and 64.95- 155.90 µg/mL for PARA.

  2. Analytic Methods for Cosmological Likelihoods

    OpenAIRE

    Taylor, A. N.; Kitching, T. D.

    2010-01-01

    We present general, analytic methods for Cosmological likelihood analysis and solve the "many-parameters" problem in Cosmology. Maxima are found by Newton's Method, while marginalization over nuisance parameters, and parameter errors and covariances are estimated by analytic marginalization of an arbitrary likelihood function with flat or Gaussian priors. We show that information about remaining parameters is preserved by marginalization. Marginalizing over all parameters, we find an analytic...

  3. Optimisation and validation of analytical methods for the simultaneous extraction of antioxidants: application to the analysis of tomato sauces.

    Science.gov (United States)

    Motilva, Maria-José; Macià, Alba; Romero, Maria-Paz; Labrador, Agustín; Domínguez, Alba; Peiró, Lluís

    2014-11-15

    In the present study, simultaneous extraction of natural antioxidants (phenols and carotenoids) in complex matrices, such as tomato sauces, is presented. The tomato sauce antioxidant compounds studied were the phenolics hydroxytyrosol, from virgin olive oil, quercetin and its derivatives, from onions, and quercetin-rutinoside as well as the carotenoid, lycopene (cis and trans), from tomatoes. These antioxidant compounds were extracted simultaneously with n-hexane/acetone/ethanol (50/25/25, v/v/v). The phenolics were analysed by ultra-performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS), and lycopene (cis- and trans-forms) was analysed using high-performance liquid chromatography coupled to a diode array detector (HPLC-DAD). After studying the parameters of these methods, they were applied to the analysis of virgin olive oil, fresh onion, tomato concentrate and tomato powder, and commercial five tomato sauces. Subsequently, the results obtained in our laboratory were compared with those from the Gallina Blanca Star Group laboratory.

  4. Validation of analytical method to calculate the concentration of conjugated monoclonal antibody; Validacao de metodo analitico para calculo de concentracao de anticorpo monoclonal conjugado

    Energy Technology Data Exchange (ETDEWEB)

    Alcarde, Lais F.; Massicano, Adriana V.F.; Oliveira, Ricardo S.; Araujo, Elaine B. de, E-mail: lais_alcarde@hotmail.com [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2013-07-01

    The objective of this study was to develop a quantitative analytical method using high performance liquid chromatography (HPLC) to determine the antibody concentration in conjunction with bifunctional chelator. Assays were performed using a high performance liquid chromatograph, and the following conditions were used: flow rate of 1 mL / min, 15 min run time, 0.2 M sodium phosphate buffer pH 7.0 as the mobile phase and column of molecular exclusion BioSep SEC S-3000 (300 x 7.8 mm, 5 μM - Phenomenex). The calibration curve was obtained with AcM diluted in 0.2 M sodium phosphate buffer pH 7.0 by serial dilution, yielding the concentrations: 400 μg/mL, 200 μg/mL, 100 μg/mL, 50 μg/mL, 25 μg/mL and 12.5 μg/mL. From the calibration curve calculated the equation of the line and with it the concentration of the immunoconjugate. To ensure the validity of the method accuracy and precision studies were conducted. The accuracy test consisted in the evaluation of 3 samples of known concentration, being this test performed with low concentrations (50 μg/mL), medium (100 μg/mL) and high (200 μg/mL). The precision test consisted of 3 consecutive measurements of one sample of known concentration, subject to the conditions set forth above for the other tests. The correlation coefficient of the standard curve was greater than 97%, the accuracy was satisfactory at low concentrations as well as accuracy. The method was validated by showing it for the accurate and precise determination of the concentration of the immunoconjugate. Furthermore, this assay was found to be extremely important, because using the correct mass of the protein, the radiochemical purity of the radioimmunoconjugate was above 95% in all studies.

  5. Fast and simple procedure for fractionation of zinc in soil using an ultrasound probe and FAAS detection. Validation of the analytical method and evaluation of the uncertainty budget.

    Science.gov (United States)

    Leśniewska, Barbara; Kisielewska, Katarzyna; Wiater, Józefa; Godlewska-Żyłkiewicz, Beata

    2016-01-01

    A new fast method for determination of mobile zinc fractions in soil is proposed in this work. The three-stage modified BCR procedure used for fractionation of zinc in soil was accelerated by using ultrasounds. The working parameters of an ultrasound probe, a power and a time of sonication, were optimized in order to acquire the content of analyte in soil extracts obtained by ultrasound-assisted sequential extraction (USE) consistent with that obtained by conventional modified Community Bureau of Reference (BCR) procedure. The content of zinc in extracts was determined by flame atomic absorption spectrometry. The developed USE procedure allowed for shortening the total extraction time from 48 h to 27 min in comparison to conventional modified BCR procedure. The method was fully validated, and the uncertainty budget was evaluated. The trueness and reproducibility of the developed method was confirmed by analysis of certified reference material of lake sediment BCR-701. The applicability of the procedure for fast, low costs and reliable determination of mobile zinc fraction in soil, which may be useful for assessing of anthropogenic impacts on natural resources and environmental monitoring purposes, was proved by analysis of different types of soil collected from Podlaskie Province (Poland).

  6. Analytic Methods in Investigative Geometry.

    Science.gov (United States)

    Dobbs, David E.

    2001-01-01

    Suggests an alternative proof by analytic methods, which is more accessible than rigorous proof based on Euclid's Elements, in which students need only apply standard methods of trigonometry to the data without introducing new points or lines. (KHR)

  7. ANALYTICAL METHOD DEVELOPMENT AND VALIDATION FOR THE ESTIMATION OF FAROPENEM IN BULK AND PHARMACEUTICAL FORMULATION USING THE RP-HPLC METHOD

    Directory of Open Access Journals (Sweden)

    Iffath Rizwana

    2012-12-01

    Full Text Available A simple, specific and accurate reverse phase high performance liquid chromatographic method was developed for the determination Faropenem in Bulk and pharmaceutical dosage form. The column used was Symmetry C18 (4.6 x 150mm, 5 m, Make: ODS or equivalent in isocratic mode, with mobile phase containing phosphate buffer adjusted the pH-4.0 with orthophosphoric acid and Acetonitrile in the ratio (70:30%v/v the flow rate was 0.9 mL/ min and eluents was monitored at 317 nm. The retention time Faropenem was 3.051 min, respectively. The linearity for Faropenem was in the range of 40-120 µg/ml respectively. The recovery of Faropenem was found to be 100.1%, respectively. The proposed method was validated and successfully applied to the estimation of Faropenem in tablet dosage form.

  8. How composition methods are developed and validated.

    Science.gov (United States)

    Rogers, Hilary A

    2013-09-04

    Method validation is a critical prerequisite to performing analytical methods in the laboratory. A given analytical method is validated for a specific matrix or matrices. If the matrix to be tested is not included in the original scope of method validation, a validation must be performed to determine if the method is applicable to that particular matrix. A number of organizations, such as AOAC and ISO, publish peer-reviewed methods for cross-industry matrices, whereas others, such as AOCS and AACC, are focused on specific industry segments (fats/oils and cereal grains). When no validated method is available for the analyte of interest, method development and validation must first be performed to ensure that correct identification and quantification of the analyte are being observed and measured. Development of a new method requires an understanding of the chemistry and properties of the analyte to be tested, as well as the various types of instrumentation currently available. Method development and improvement is a continuous process, as technology advances and new instrumentation and techniques become available. This paper addresses some of the decisions related to method development but will primarily focus on validation as it applies to compositional testing of foods, crops, and commodities, the factors that determine method selection, and how extensive the validation need be.

  9. Validation of an Analytical Method for Determination of 13 priority polycyclic aromatic hydrocarbons in mineral water using dispersive liquid-liquid microextraction and GC-MS

    Science.gov (United States)

    Sadeghi, Ramezan; Kobarfard, Farzad; Yazdanpanah, Hassan; Eslamizad, Samira; Bayat, Mitra

    2016-01-01

    Dispersive liquid-liquid microextraction (DLLME) combined with gas chromatography–mass spectrometry (GC–MS) was used for the extraction and determination of 13 polycyclic aromatic hydrocarbons (PAHs) in mineral water samples. In this procedure, the suitable combination of extraction solvent (500 µL chloroform) and disperser solvent (1000 µL acetone) were quickly injected into the water sample (10.00 mL) by Hamilton syringe. After centrifugation, 500 µL of the lower organic phase was dried under a gentle stream of nitrogen, re-dissolved in chloroform and injected into GC-MS. Chloroform and acetone were found to be the best extraction and disperser solvent, respectively. Validation of the method was performed using spiked calibration curves. The enrichment factor ranged from 93 to 129 and the recovery ranged from 71 to 90%. The linear ranges for all the PAHs were 0.10-2.80 ngmL-1. The relative standard deviations (RSDs) of PAHs in water by using anthracene-d10 as internal standard, were in the range of 4-11% for most of the analytes (n = 3). Limit of detection (LOD) for different PAHs were between 0.03 and 0.1 ngmL-1. The method was successfully applied for the analysis of PAHs in mineral water samples collected from Tehran. PMID:27610156

  10. Salbutamol extraction from urine and its stability in different solutions: identification of methylation products and validation of a quantitative analytical method.

    Science.gov (United States)

    Garrido, Bruno Carius; Silva, Mayra Leal Chrisóstomo; Borges, Ricardo Moreira; Padilha, Monica Costa; de Aquino Neto, Francisco Radler

    2013-12-01

    Salbutamol is commonly used in asthma treatment, being considered a short-effect bronchodilator. This drug poses special interest in certain fields of chemical analysis, such as food, clinical and doping analyses, in which it needs to be analyzed with quantitative precision and accuracy. Salbutamol, however, is known to degrade under certain conditions and this is critical if quantitative results must be generated. The present work aimed to investigate salbutamol extraction from urine samples, to determine whether salbutamol is unstable in other solvents as well as in urine samples, to elucidate the structures of the possible degradation products and to validate an analytical method using the extraction procedure evaluated. Stability investigations were performed in urine at different pH values, in methanol and acetone at different temperatures. Semi-preparative liquid chromatography was performed for the isolation of degradation products, and gas chromatography coupled to mass spectrometry as well as nuclear magnetic resonance were used for identification. Three unreported methylation products were detected in methanolic solutions and had their structures elucidated. Urine samples showed a reduction in salbutamol concentration of up to 25.8% after 5 weeks. These results show that special care must be taken regarding salbutamol quantitative analyses, since degradation either in standard solutions or in urine could lead to incorrect values.

  11. Analytical method (HPLC), validation used for identification and assay of the pharmaceutical active ingredient, Tylosin tartrate for veterinary use and its finite product Tilodem 50, hydrosoluble powder

    OpenAIRE

    2010-01-01

    In SC DELOS IMPEX ’96 SRL the quality of the active pharmaceutical ingredient (API) for the finite product Tilodem 50 - hydrosoluble powder was acomkplished in the respect of last European Pharmacopoeia.The method for analysis used in this purpose was the compendial method „Tylosin tartrate for veterinary use” in EurPh. in vigour edition and represent a variant developed and validation „in house”.The parameters which was included in the methodology validation for chromatographic method are th...

  12. Determination of serum levels of imatinib mesylate in patients with chronic myeloid leukemia: validation and application of a new analytical method to monitor treatment compliance

    Directory of Open Access Journals (Sweden)

    Vinícius Marcondes Rezende

    2013-01-01

    Full Text Available OBJECTIVE: The goal of this study was to monitor imatinib mesylate therapeutically in the Tumor Biology Laboratory, Department of Hematology and Hemotherapy, Hospital das Clínicas, Faculdade de Medicina, Universidade de São Paulo (USP. A simple and sensitive method to quantify imatinib and its metabolite (CGP74588 in human serum was developed and fully validated in order to monitor treatment compliance. METHODS: The method used to quantify these compounds in serum included protein precipitation extraction followed by instrumental analysis using high performance liquid chromatography coupled with mass spectrometry. The method was validated for several parameters, including selectivity, precision, accuracy, recovery and linearity. RESULTS: The parameters evaluated during the validation stage exhibited satisfactory results based on the Food and Drug Administration and the Brazilian Health Surveillance Agency (ANVISA guidelines for validating bioanalytical methods. These parameters also showed a linear correlation greater than 0.99 for the concentration range between 0.500 µg/mL and 10.0 µg/mL and a total analysis time of 13 minutes per sample. This study includes results (imatinib serum concentrations for 308 samples from patients being treated with imatinib mesylate. CONCLUSION: The method developed in this study was successfully validated and is being efficiently used to measure imatinib concentrations in samples from chronic myeloid leukemia patients to check treatment compliance. The imatinib serum levels of patients achieving a major molecular response were significantly higher than those of patients who did not achieve this result. These results are thus consistent with published reports concerning other populations.

  13. The validation of an analytical method for sulfentrazone residue determination in soil using liquid chromatography and a comparison of chromatographic sensitivity to millet as a bioindicator species.

    Science.gov (United States)

    de Oliveira, Marcelo Antonio; Pires, Fábio Ribeiro; Ferraço, Mariana; Belo, Alessandra Ferreira

    2014-07-28

    Commonly used herbicides, such as sulfentrazone, pose the risk of soil contamination due to their persistence, bioaccumulation and toxicity. Phytoremediation by green manure species has been tested using biomarkers, but analytical data are now required to confirm the extraction of sulfentrazone from soil. Thus, the present work was carried out to analyze sulfentrazone residues in soil based on liquid chromatography with a comparison of these values to the sensitivity of the bioindicator Pennisetum glaucum. The soil samples were obtained after cultivation of Crotalaria juncea and Canavalia ensiformis at four seeding densities and with three doses of sulfentrazone. The seedlings were collected into pots, at two different depths, after 75 days of phytoremediator sowing and then were used to determine the herbicide persistence in the soil. A bioassay with P. glaucum was carried out in the same pot. High-performance liquid chromatography (HPLC), using UV-diode array detection (HPLC/UV-DAD), was used to determine the herbicide residues. The HPLC determination was optimized and validated according to the parameters of precision, accuracy, linearity, limit of detection and quantification, robustness and specificity. The bioindicator P. glaucum was more sensitive to sulfentrazone than residue determination by HPLC. Changes in sulfentrazone concentration caused by green manure phytoremediation were accurately identified by the bioindicator. However, a true correlation between the size of the species and the analyte content was not identified.

  14. The Validation of an Analytical Method for Sulfentrazone Residue Determination in Soil Using Liquid Chromatography and a Comparison of Chromatographic Sensitivity to Millet as a Bioindicator Species

    Directory of Open Access Journals (Sweden)

    Marcelo Antonio de Oliveira

    2014-07-01

    Full Text Available Commonly used herbicides, such as sulfentrazone, pose the risk of soil contamination due to their persistence, bioaccumulation and toxicity. Phytoremediation by green manure species has been tested using biomarkers, but analytical data are now required to confirm the extraction of sulfentrazone from soil. Thus, the present work was carried out to analyze sulfentrazone residues in soil based on liquid chromatography with a comparison of these values to the sensitivity of the bioindicator Pennisetum glaucum. The soil samples were obtained after cultivation of Crotalaria juncea and Canavalia ensiformis at four seeding densities and with three doses of sulfentrazone. The seedlings were collected into pots, at two different depths, after 75 days of phytoremediator sowing and then were used to determine the herbicide persistence in the soil. A bioassay with P. glaucum was carried out in the same pot. High-performance liquid chromatography (HPLC, using UV-diode array detection (HPLC/UV-DAD, was used to determine the herbicide residues. The HPLC determination was optimized and validated according to the parameters of precision, accuracy, linearity, limit of detection and quantification, robustness and specificity. The bioindicator P. glaucum was more sensitive to sulfentrazone than residue determination by HPLC. Changes in sulfentrazone concentration caused by green manure phytoremediation were accurately identified by the bioindicator. However, a true correlation between the size of the species and the analyte content was not identified.

  15. Consistency of FMEA used in the validation of analytical procedures.

    Science.gov (United States)

    Oldenhof, M T; van Leeuwen, J F; Nauta, M J; de Kaste, D; Odekerken-Rombouts, Y M C F; Vredenbregt, M J; Weda, M; Barends, D M

    2011-02-20

    In order to explore the consistency of the outcome of a Failure Mode and Effects Analysis (FMEA) in the validation of analytical procedures, an FMEA was carried out by two different teams. The two teams applied two separate FMEAs to a High Performance Liquid Chromatography-Diode Array Detection-Mass Spectrometry (HPLC-DAD-MS) analytical procedure used in the quality control of medicines. Each team was free to define their own ranking scales for the probability of severity (S), occurrence (O), and detection (D) of failure modes. We calculated Risk Priority Numbers (RPNs) and we identified the failure modes above the 90th percentile of RPN values as failure modes needing urgent corrective action; failure modes falling between the 75th and 90th percentile of RPN values were identified as failure modes needing necessary corrective action, respectively. Team 1 and Team 2 identified five and six failure modes needing urgent corrective action respectively, with two being commonly identified. Of the failure modes needing necessary corrective actions, about a third were commonly identified by both teams. These results show inconsistency in the outcome of the FMEA. To improve consistency, we recommend that FMEA is always carried out under the supervision of an experienced FMEA-facilitator and that the FMEA team has at least two members with competence in the analytical method to be validated. However, the FMEAs of both teams contained valuable information that was not identified by the other team, indicating that this inconsistency is not always a drawback.

  16. DEVELOPMENT AND VALIDATION OF ANALYTICAL METHOD FOR SIMULTANEOUS ESTIMATION OF MUPIROCIN AND MOMETASONE FUROATE IN TOPICAL FORMULATION BY RP-HPLC

    Directory of Open Access Journals (Sweden)

    Arti P. Parmar

    2015-04-01

    Full Text Available Purpose: To develop simple, precise, rapid RP-HPLC (Reverse-phase High Performance Liquid Chromatography method for estimation of marketed combination formulation of Mupirocin and Mometasone Furoate. Methods: The Chromatographic separation was achieved on a reversed-phase Phenomenax-luna C18 (250 x 4.6mm, 5 μm column using a mobile phase consisting of acetonitrile : Sodium dihydrogen phosphate buffer (pH 6.8 (70:30 v/v at a flow rate of 1 mL/min and UV detection at 240 nm. Developed methods were validated according to ICH Q2 (R1 guidelines. The methods were found to be linear between the range of 10 - 60 μg/ml for Mupirocin and 1 – 6 μg/ml for Mometasone Furoate. Results: An intra-day precision for Mupirocin was found to be 0.6788% - 0.9820% and for Mometasone Furoate 0.6758%- 0.7532%, inter-day precision for Mupirocin was found to be 0.9775% - 1.1277% for Mometasone Furoate 0.9114% - 1.0765%. Accuracy was determined by recovery studies and showed % recovery between 98 to 102%. Conclusions: A simple, accurate and precise HPLC method was developed and validated for the routine analysis of Mometasone Furoate and Mupirocin in ointment topical formulation. The results make known that the proposed method could be successfully useful for the routine analysis and quality control of pharmaceutical dosage forms containing Mometasone Furoate and Mupirocin. NOVELTY OF THE WORK - The proposed HPLC method was validated as per ICH guidelines. The drug was extracted from an ointment and there is no any interference of excipients was founded. The results of the recovery studies performed show the high degree of accuracy of the proposed method, hence proposed method will useful to routine analysis of Mometasone Furoate and Mupirocin.

  17. Risk analysis by FMEA as an element of analytical validation.

    Science.gov (United States)

    van Leeuwen, J F; Nauta, M J; de Kaste, D; Odekerken-Rombouts, Y M C F; Oldenhof, M T; Vredenbregt, M J; Barends, D M

    2009-12-05

    We subjected a Near-Infrared (NIR) analytical procedure used for screening drugs on authenticity to a Failure Mode and Effects Analysis (FMEA), including technical risks as well as risks related to human failure. An FMEA team broke down the NIR analytical method into process steps and identified possible failure modes for each step. Each failure mode was ranked on estimated frequency of occurrence (O), probability that the failure would remain undetected later in the process (D) and severity (S), each on a scale of 1-10. Human errors turned out to be the most common cause of failure modes. Failure risks were calculated by Risk Priority Numbers (RPNs)=O x D x S. Failure modes with the highest RPN scores were subjected to corrective actions and the FMEA was repeated, showing reductions in RPN scores and resulting in improvement indices up to 5.0. We recommend risk analysis as an addition to the usual analytical validation, as the FMEA enabled us to detect previously unidentified risks.

  18. Validation of an analytical method for quality control of residual solvents (n-hexane and acetone) in D-002: new active ingredient from beeswax.

    Science.gov (United States)

    Antolín, Ernesto Méndez; Quiñónez, Yaisme Balcinde; Canavaciolo, Víctor González; Cruz, Esperanza Rodríguez

    2008-07-15

    D-002 is a new natural product consisting of a mixture of aliphatic fatty alcohols, which shows antioxidant and anti-ulcer effects in experimental models. A new validated methodology for determining simultaneously residual n-hexane and acetone in D-002 using the headspace gas chromatography (HS/GC) is described. The very poor solubility of D-002 in most solvents did necessary sample preparations in solid state. Limit test conditions allowed a detection of residual n-hexane and acetone more sensitively than that recommended for such purposes in the general method of the European Pharmacopoeia. Validation assays, applied to both D-002 residual solvents, proved: suitable sensitivity; very high linearity (correlation coefficients > or =0.999, R.S.D. of slopes < or =0.8% and R.S.D. of response factors < or =5% and no biases) and accuracy (average recoveries between 94.7 and 100.1%); and precision was < or =2.1%. The method was found suitable for quality control and stability studies of this new product.

  19. 7 CFR 98.4 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 98.4 Section 98.4 Agriculture....4 Analytical methods. (a) The majority of analytical methods used by the USDA laboratories to perform analyses of meat, meat food products and MRE's are listed as follows: (1) Official Methods...

  20. 7 CFR 94.303 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.303 Section 94.303 Agriculture... POULTRY AND EGG PRODUCTS Processed Poultry Products § 94.303 Analytical methods. The analytical methods... latest edition of the Official Methods of Analysis of AOAC INTERNATIONAL, Suite 500, 481 North...

  1. 7 CFR 93.4 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.4 Section 93.4 Agriculture... PROCESSED FRUITS AND VEGETABLES Citrus Juices and Certain Citrus Products § 93.4 Analytical methods. (a) The majority of analytical methods for citrus products are found in the Official Methods of Analysis of...

  2. 7 CFR 94.103 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 94.103 Section 94.103 Agriculture... POULTRY AND EGG PRODUCTS Voluntary Analyses of Egg Products § 94.103 Analytical methods. The analytical methods used by the Science and Technology Division laboratories to perform voluntary analyses for...

  3. Analytical validation of accelerator mass spectrometry for pharmaceutical development.

    Science.gov (United States)

    Keck, Bradly D; Ognibene, Ted; Vogel, John S

    2010-03-01

    The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of (14)C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the (14)C label), stable across samples storage conditions for at least 1 year, linear over four orders of magnitude with an analytical range from 0.1 Modern to at least 2000 Modern (instrument specific). Furthermore, accuracy was excellent (between 1 and 3%), while precision expressed as coefficient of variation was between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of (14)C, respectively (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with (14)C corresponds to 30 fg equivalents. Accelerator mass spectrometry provides a sensitive, accurate and precise method of measuring drug compounds in biological matrices.

  4. Comparison and validation of 2 analytical methods for the determination of free fatty acids in dairy products by gas chromatography with flame ionization detection.

    Science.gov (United States)

    Mannion, David T; Furey, Ambrose; Kilcawley, Kieran N

    2016-07-01

    Accurate quantification of free fatty acids (FFA) in dairy products is important for quality control, nutritional, antimicrobial, authenticity, legislative, and flavor purposes. In this study, the performance of 2 widely used gas chromatographic flame ionization detection methods for determination of FFA in dairy products differing in lipid content and degree of lipolysis were evaluated. We used a direct on-column approach where the isolated FFA extract was injected directly and a derivatization approach where the FFA were esterified in the injector to methyl esters using tetramethylammonium hydroxide as a catalyst. A comprehensive validation was undertaken to establish method linearity, limits of detection, limits of quantification, accuracy, and precision. Linear calibrations of 3 to 700mg/L (R(2)>0.999) and 20 to 700mg/L (R(2)>0.997), and limits of detection and limits of quantification of 0.7 and 3mg/L and 5 and 20mg/L were obtained for the direct injection on-column and the derivatization method, respectively. Intraday precision of 1.5 to 7.2% was obtained for both methods. The direct injection on-column method had the lower levels of limits of detection and quantification, because FFA are directly injected onto the GC as opposed to the split injection used in the derivatization method. However, the direct injection on-column method experienced accumulative column phase deterioration and irreversible FFA absorption because of the acidic nature of the injection extract, which adversely affected method robustness and the quantification of some longer chain FFA. The derivatization method experienced issues with quantification of butyric acid at low concentrations because of coelution with the injection solvent peak, loss of polyunsaturated FFA due to degradation by tetramethylammonium hydroxide, and the periodic emergence of by-product peaks of the tetramethylammonium hydroxide reaction that interfered with the quantification of some short-chain FFA. The

  5. Implementation of QbD Approach to the Analytical Method Development and Validation for the Estimation of Propafenone Hydrochloride in Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    Monika L. Jadhav

    2013-01-01

    Full Text Available Chromatographic and spectrophotometric methods were developed according to Quality by Design (QbD approach as per ICH Q8(R2 guidelines for estimation of propafenone hydrochloride in tablet dosage form. QbD approach was carried out by varying various parameters and these variable parameters were designed into Ishikawa diagram. The critical parameters were determined by using principal component analysis as well as by observation. Estimated critical parameters in HPTLC method include solvent methanol, mode of detection absorbance, precoated aluminium backed TLC plate (10 cm 10 cm, wavelength: 250 nm, saturation time: 20 min, band length: 8 mm, solvent front: 70 mm, volume of mobile phase: 5 mL, type of chamber: 10 cm 10 cm, scanning time: 10 min, and mobile phase methanol : ethyl acetate : triethylamine (1.5 : 3.5 : 0.4 v/v/v. Estimated critical parameters in zero order spectrophotometric method were solvent methanol, sample preparation tablet, wavelength: 247.4 nm, slit width: 1.0, scan speed medium, and sampling interval: 0.2, and for first order derivative spectrophotometric method it was scaling factor: 5 and delta lambda 4. The above methods were validated according to ICH Q2(R1 guidelines. Proposed methods can be used for routine analysis of propafenone hydrochloride in tablet dosage form as they were found to be robust and specific.

  6. Development and validation of new analytical methods for simultaneous estimation of Drotaverine hydrochloride in combination with Omeprazole in a pharmaceutical dosage form

    Directory of Open Access Journals (Sweden)

    Smita Sharma

    2017-02-01

    Full Text Available A rapid and precise method (in accordance with ICH guidelines is developed for the quantitative simultaneous determination of Drotaverine hydrochloride and Omeprazole in a combined pharmaceutical dosage form. Three methods are described for the simultaneous determination of Drotaverine hydrochloride and Omeprazole in a binary mixture. The first method was based on UV-Spectrophotometric determination of two drugs, using Vierordt!s simultaneous equation method. It involves absorbance measurement at 226.8 nm (λmax of Drotaverine hydrochloride and 269.4 nm (λmax of Omeprazole in methanol; linearity was obtained in the range of 5–30 μg ml−1 for both the drugs. The second method was based on HPLC separation of the two drugs using potassium dihydrogen phosphate buffer pH 5.0: Acetonitrile: Triethylamine (60:40:0.5, v/v as a mobile phase. Areas were recorded at 260 nm for both the drugs and retention time was found to be 2.71 min. and 3.87 min for Drotaverine hydrochloride and Omeprazole, respectively at 1.0 mL/min flow rate. The selected chromatographic conditions were found to determine Drotaverine hydrochloride and Omeprazole quantitatively in a combined dosage form without any physical separation. The method has been validated for linearity, accuracy and precision. Linearity was found over the range of 5–30 μg mL−1 for both drugs. The third method was based on HPTLC method for simultaneous quantification of these compounds in pharmaceutical dosage forms. Precoated silica gel 60 F254 plate was used as stationary phase. The separation was carried out using Glacial acetic acid:Cyclohexane:Methanol:(80:15:5 v/v/v as mobile phase. The proposed method was found to be fast, accurate, precise, reproducible and rugged and can be used for a simultaneous analysis of these drugs in combined formulations.

  7. Synthesis of trans- and cis-4'-hydroxylomustine and development of validated analytical method for lomustine and trans- and cis-4'-hydroxylomustine in canine plasma.

    Science.gov (United States)

    Dirikolu, L; Chakkath, T; Fan, T; Mente, Nolan R

    2009-01-01

    In veterinary medicine, lomustine has been successfull used primarily for the treatment of resistant lymphoma and also for the treatment of mast cell tumors, intracranial meningioma, epitheliotropic lymphoma, and histiocytic sarcoma in dogs either alone or in combination with other chemotherapeutic agents. Even though lomustine is commonly used in dogs primarily for the treatment of resistant lymphoma, there is no pharmacokinetics information available regarding this compound in dogs. In the present study, we developed and validated a simple high-performance liquid chromatography (HPLC) method with a one-step liquid-liquid extraction procedure to detect and quantify lomustine and its two monohydroxylated metabolites (trans- and cis-4'-hydroxylomustine) in canine plasma for future pharmacokinetic studies. The HPLC-diode-array detection method reported here readily detects lomustine, cis-4'-hydroxylomustine, and trans-4'-hydroxylomustine in canine plasma with a limit of detection of lomustine, cis-4'-hydroxylomustine, and trans-4'-hydroxylomustine in plasma of about 10 ng/120 microL, 5 ng/120 microL, and 5 ng/120 microL, respectively. The mean extraction efficiency values for lomustine, cis-4'-hydroxylomustine, and trans-4'-hydroxylomustine were 73%, 90%, and 89%, respectively, from canine plasma samples on HPLC. The present study also provides stability information about lomustine and its two monohydroxylated metabolites in canine plasma and methanol solution stored at various conditions.

  8. Analytical method development and validation of simultaneous estimation of rabeprazole, pantoprazole, and itopride by reverse-phase high-performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Senthamil Selvan Perumal

    2014-12-01

    Full Text Available A simple, selective, rapid, and precise reverse-phase high-performance liquid chromatography (RP-HPLC method for the simultaneous estimation of rabeprazole (RP, pantoprazole (PP, and itopride (IP has been developed. The compounds were well separated on a Phenomenex C18 (Luna column (250 mm × 4.6 mm, dp = 5 μm with C18 guard column (4 mm × 3 mm × 5 μm with a mobile phase consisting of buffer containing 10 mM potassium dihydrogen orthophosphate (adjusted to pH 6.8: acetonitrile (70:30 v/v at a flow rate of 1.0 mL/min and ultraviolet detection at 288 nm. The retention time of RP, PP, and IP were 5.35, 7.92, and 11.16 minutes, respectively. Validation of the proposed method was carried out according to International Conference on Harmonisation (ICH guidelines. Linearity range was obtained for RP, PP, and IP over the concentration range of 2.5–25, 1–30, and 3–35 μg/mL and the r2 values were 0.994, 0.978, and 0.991, respectively. The calculated limit of detection (LOD values were 1, 0.3, and 1 μg/mL and limit of quantitation (LOQ values were 2.5, 1, and 3 μg/mL for RP, PP, and IP correspondingly. Thus, the current study showed that the developed reverse-phase liquid chromatography method is sensitive and selective for the estimation of RP, PP, and IP in combined dosage form.

  9. Development and validation of an ESI-LC-MS/MS method for simultaneous identification and quantification of 24 analytes of forensic relevance in vitreous humour, whole blood and plasma.

    Science.gov (United States)

    Arora, Beauty; Velpandian, Thirumurthy; Saxena, Rohit; Lalwani, Sanjeev; Dogra, T D; Ghose, Supriyo

    2016-01-01

    Detection and quantification of drugs from various biological matrices are of immense importance in forensic toxicological analysis. Despite the various reported methods, development of a new method for the detection and quantification of drugs is still an active area of research. However, every method and biological matrix has its own limitation, which further encourage forensic toxicologists to develop new methods and to explore new matrices for the analysis of drugs. In this study, an electrospray ionization-liquid chromatograph-tandem mass spectrometry (ESI-LC-MS/MS) method is developed and validated for simultaneous identification and quantification of 24 drugs of forensic relevance in various body fluids, namely, whole blood, plasma and vitreous humour. The newly developed method has been validated for intra-day and inter-day accuracy, precision, selectivity and sensitivity. Absolute recovery shows a mean of 84.5, 86.2, and 103% in the vitreous humour, whole blood and plasma respectively, which is suitable for the screening procedure. Further, the absolute matrix effect (AME) shows a mean of 105, 96.5, and 109% in the vitreous humour, whole blood and plasma, respectively. In addition, to examine the practical utility of this method, it has been applied for screening of drugs in post-mortem samples of the vitreous humour, whole blood and plasma collected at autopsy from ten cadavers. Experimental results show that the newly developed method is well applicable for screening of analytes in all the three matrices.

  10. Analytical mechanics methods for solving Whittaker equations

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The purpose of this paper is to study the solution of the celebrated Whittaker equations by using analytical mechanics methods, including the Lagrange-Noether method, Hamilton-Poisson method and potential integral method.

  11. 40 CFR 141.89 - Analytical methods.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Analytical methods. 141.89 Section 141...) NATIONAL PRIMARY DRINKING WATER REGULATIONS Control of Lead and Copper § 141.89 Analytical methods. (a... shall be conducted with the methods in § 141.23(k)(1). (1) Analyses for alkalinity,...

  12. Consistency of FMEA used in the validation of analytical procedures

    DEFF Research Database (Denmark)

    Oldenhof, M.T.; van Leeuwen, J.F.; Nauta, Maarten

    2011-01-01

    In order to explore the consistency of the outcome of a Failure Mode and Effects Analysis (FMEA) in the validation of analytical procedures, an FMEA was carried out by two different teams. The two teams applied two separate FMEAs to a High Performance Liquid Chromatography-Diode Array Detection......-Mass Spectrometry (HPLC-DAD-MS) analytical procedure used in the quality control of medicines. Each team was free to define their own ranking scales for the probability of severity (S), occurrence (O), and detection (D) of failure modes. We calculated Risk Priority Numbers (RPNs) and we identified the failure modes...

  13. Risk analysis of analytical validations by probabilistic modification of FMEA

    DEFF Research Database (Denmark)

    Barends, D.M.; Oldenhof, M.T.; Vredenbregt, M.J.

    2012-01-01

    Risk analysis is a valuable addition to validation of an analytical chemistry process, enabling not only detecting technical risks, but also risks related to human failures. Failure Mode and Effect Analysis (FMEA) can be applied, using a categorical risk scoring of the occurrence, detection...... and severity of failure modes, and calculating the Risk Priority Number (RPN) to select failure modes for correction. We propose a probabilistic modification of FMEA, replacing the categorical scoring of occurrence and detection by their estimated relative frequency and maintaining the categorical scoring...... of undetected failure mode(s) can be estimated quantitatively, for each individual failure mode, for a set of failure modes, and the full analytical procedure....

  14. Alternative methods in toxicology: pre-validated and validated methods.

    Science.gov (United States)

    Kandárová, Helena; Letašiová, Silvia

    2011-09-01

    The development of alternative methods to animal experimentation has progressed rapidly over the last 20 years. Today, in vitro and in silico methods have an important role in the hazard identification and assessment of toxicology profile of compounds. Advanced alternative methods and their combinations are also used for safety assessment of final products. Several alternative methods, which were scientifically validated and accepted by competent regulatory bodies, can be used for regulatory toxicology purposes, thus reducing or fully replacing living animals in toxicology experimentation. The acceptance of the alternative methods as valuable tools of modern toxicology has been recognized by regulators, including OECD, FDA and EPA.This paper provides a brief overview of the topic "alternative methods in toxicology" and focuses on pre-validated and validated alternative methods and their position in the modern toxicology.

  15. Risk analysis of analytical validations by probabilistic modification of FMEA.

    Science.gov (United States)

    Barends, D M; Oldenhof, M T; Vredenbregt, M J; Nauta, M J

    2012-05-01

    Risk analysis is a valuable addition to validation of an analytical chemistry process, enabling not only detecting technical risks, but also risks related to human failures. Failure Mode and Effect Analysis (FMEA) can be applied, using a categorical risk scoring of the occurrence, detection and severity of failure modes, and calculating the Risk Priority Number (RPN) to select failure modes for correction. We propose a probabilistic modification of FMEA, replacing the categorical scoring of occurrence and detection by their estimated relative frequency and maintaining the categorical scoring of severity. In an example, the results of traditional FMEA of a Near Infrared (NIR) analytical procedure used for the screening of suspected counterfeited tablets are re-interpretated by this probabilistic modification of FMEA. Using this probabilistic modification of FMEA, the frequency of occurrence of undetected failure mode(s) can be estimated quantitatively, for each individual failure mode, for a set of failure modes, and the full analytical procedure.

  16. 7 CFR 91.23 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ...-2417. (i) Standard Analytical Methods of the Member Companies of Corn Industries Research Foundation... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 91.23 Section 91.23 Agriculture Regulations of the Department of Agriculture (Continued) AGRICULTURAL MARKETING SERVICE...

  17. 7 CFR 93.13 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... manuals: (a) Approved Methods of the American Association of Cereal Chemists (AACC), American Association... 7 Agriculture 3 2010-01-01 2010-01-01 false Analytical methods. 93.13 Section 93.13 Agriculture... PROCESSED FRUITS AND VEGETABLES Peanuts, Tree Nuts, Corn and Other Oilseeds § 93.13 Analytical...

  18. Validation of a multi-analyte HPLC-DAD method for determination of uric acid, creatinine, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid and 2-methylhippuric acid in human urine.

    Science.gov (United States)

    Remane, Daniela; Grunwald, Soeren; Hoeke, Henrike; Mueller, Andrea; Roeder, Stefan; von Bergen, Martin; Wissenbach, Dirk K

    2015-08-15

    During the last decades exposure sciences and epidemiological studies attracts more attention to unravel the mechanisms for the development of chronic diseases. According to this an existing HPLC-DAD method for determination of creatinine in urine samples was expended for seven analytes and validated. Creatinine, uric acid, homovanillic acid, niacinamide, hippuric acid, indole-3-acetic acid, and 2-methylhippuric acid were separated by gradient elution (formate buffer/methanol) using an Eclipse Plus C18 Rapid Resolution column (4.6mm×100mm). No interfering signals were detected in mobile phase. After injection of blank urine samples signals for the endogenous compounds but no interferences were detected. All analytes were linear in the selected calibration range and a non weighted calibration model was chosen. Bias, intra-day and inter-day precision for all analytes were below 20% for quality control (QC) low and below 10% for QC medium and high. The limits of quantification in mobile phase were in line with reported reference values but had to be adjusted in urine for homovanillic acid (45mg/L), niacinamide 58.5(mg/L), and indole-3-acetic acid (63mg/L). Comparison of creatinine data obtained by the existing method with those of the developed method showing differences from -120mg/L to +110mg/L with a mean of differences of 29.0mg/L for 50 authentic urine samples. Analyzing 50 authentic urine samples, uric acid, creatinine, hippuric acid, and 2-methylhippuric acid were detected in (nearly) all samples. However, homovanillic acid was detected in 40%, niacinamide in 4% and indole-3-acetic acid was never detected within the selected samples.

  19. Study of hydroxymethylfurfural and furfural formation in cakes during baking in different ovens, using a validated multiple-stage extraction-based analytical method.

    Science.gov (United States)

    Petisca, Catarina; Henriques, Ana Rita; Pérez-Palacios, Trinidad; Pinho, Olívia; Ferreira, Isabel M P L V O

    2013-12-15

    A procedure for extraction of hydroxymethylfurfural (HMF) and furfural from cakes was validated. Higher yield was achieved by multiple step extraction with water/methanol (70/30) and clarification with Carrez I and II reagents. Oven type and baking time strongly influenced HMF, moisture and volatile profile of model cakes, whereas furfural content was not significantly affected. No correlation was found between these parameters. Baking time influenced moisture and HMF formation in cakes from traditional and microwave ovens but not in steam oven cakes. Significant moisture decrease and HMF increase (3.63, 9.32, and 41.9 mg kg(-1)dw at 20, 40 and 60 min, respectively) were observed during traditional baking. Cakes baked by microwave also presented a significant increase of HMF (up to 16.84 mg kg(-1)dw at 2.5 min). Steam oven cakes possessed the highest moisture content and no significant differences in HMF and furfural. This oven is likely to form low HMF and furfural, maintaining cake moisture and aroma compounds.

  20. Alternative methods in toxicology: pre-validated and validated methods

    OpenAIRE

    2011-01-01

    The development of alternative methods to animal experimentation has progressed rapidly over the last 20 years. Today, in vitro and in silico methods have an important role in the hazard identification and assessment of toxicology profile of compounds. Advanced alternative methods and their combinations are also used for safety assessment of final products. Several alternative methods, which were scientifically validated and accepted by competent regulatory bodies, can be used for regulatory ...

  1. Validation of an analytical method for the determination of valsartan in human plasma by HPLC/UV with addition standard using losartan as an internal standard.

    Directory of Open Access Journals (Sweden)

    Milena Pérez

    2009-11-01

    Full Text Available Introducción: El concepto de validación se refiere a la evaluación estadística de los resultados obtenidos en la aplicación de técnicas analíticas, mediante pruebas convenientemente documentadas y demostrativas de que un método es lo suficientemente fiable a fin de producir el resultado previsto bajo condiciones definidas, como son: sistema analítico, intervalo de concentración, infraestructura y talento humano. Objetivo: Describir el proceso de validación del método analítico para la cuantificación de valsartán en plasma humano por HPLC-UV y su aplicación en estudios farmacocinéticos, de biodisponibilidad y bioequivalencia de medicamentos que contengan valsartán como principio activo. Metodología: Se desarrolló un método para la detección y cuantificación de valsartán en plasma humano, con elución isocrática por cromatografía líquida de fase reversa, con detección ultravioleta a 265 nm, mediante el método de adición de estándar. Se utilizó losartán como estándar interno. El método implica una extracción en fase sólida de los principios activos (valsartán y losartán con cartuchos C8. La separación se realizó en una columna C18 en fase reversa y la fase móvil fue una mezcla de acetonitrilo: buffer fosfato  (45:55 v/v ajustado a pH 2.7±0.1 con ácido fosfórico concentrado. El método se validó en el rango de concentraciones de 0.05 a 20 µg/ml con adición de estándar de valsartán de 2.5 µg/ml. Resultados y conclusiones: La curva de calibración fue lineal en el rango de concentraciones establecido. Se evaluó la reproducibilidad, estabilidad y porcentaje de recuperación del método. El método para determinar el valsartán en plasma humano por HPLC/UV fue preciso y exacto con un límite de cuantificación de 1.485 µg/ml. Este método fue suficientemente sensible para su aplicación en estudios farmacocinéticos de valsartán.

  2. Comparison between external and internal standard calibration in the validation of an analytical method for 1-hydroxypyrene in human urine by high-performance liquid chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Pigini, D; Cialdella, A M; Faranda, P; Tranfo, G

    2006-01-01

    1-Hydroxypyrene is a metabolite of pyrene, a member of the class of polycyclic aromatic hydrocarbons (PAHs) whose toxic properties in some cases include carcinogenicity. The determination of 1-hydroxypyrene in human urine is used as a biological indicator for exposure to PAHs, which is related to the combustion of organic materials, like smoking, living in urban environments, and eating grilled or smoked food. The determination of 1-hydroxypyrene by high-performance liquid chromatography (HPLC) with fluorescence detection has very good sensitivity but it is not highly specific: this can reduce accuracy in the quantitative determination of low levels of analyte in a complex matrix like urine. An HPLC method that uses triple quadrupole mass detection has been validated with the objective both to improve the signal-to-noise (S/N) ratio and to achieve the maximum specificity for the analyte in those urine samples that are richer in possible inteferents. The calibration range for 1-hydroxypyrene is from 0.005-0.1 microg/L in the urine of non-smoking healthy volunteers. After solid-phase extraction, samples were analyzed by HPLC/tandem mass spectrometry (MS/MS) in the multiple reaction monitoring (MRM) mode. In order to obtain reliable results quantitative analysis must be performed by means of the internal standard method (we used deuterium-labelled 1-hydroxypyrene): the method accuracy is not less than 85%. The S/N ratio at a concentration of 0.1 microg/L is about 10, and therefore this can be considered the lowest limit of quantitation. The method performance does not change if urine samples are measured using a calibration curve prepared in methanol, thus reducing the time of analysis and costs.

  3. A New Method to Study Analytic Inequalities

    Directory of Open Access Journals (Sweden)

    Xiao-Ming Zhang

    2010-01-01

    Full Text Available We present a new method to study analytic inequalities involving n variables. Regarding its applications, we proved some well-known inequalities and improved Carleman's inequality.

  4. Prioritizing pesticide compounds for analytical methods development

    Science.gov (United States)

    Norman, Julia E.; Kuivila, Kathryn M.; Nowell, Lisa H.

    2012-01-01

    The U.S. Geological Survey (USGS) has a periodic need to re-evaluate pesticide compounds in terms of priorities for inclusion in monitoring and studies and, thus, must also assess the current analytical capabilities for pesticide detection. To meet this need, a strategy has been developed to prioritize pesticides and degradates for analytical methods development. Screening procedures were developed to separately prioritize pesticide compounds in water and sediment. The procedures evaluate pesticide compounds in existing USGS analytical methods for water and sediment and compounds for which recent agricultural-use information was available. Measured occurrence (detection frequency and concentrations) in water and sediment, predicted concentrations in water and predicted likelihood of occurrence in sediment, potential toxicity to aquatic life or humans, and priorities of other agencies or organizations, regulatory or otherwise, were considered. Several existing strategies for prioritizing chemicals for various purposes were reviewed, including those that identify and prioritize persistent, bioaccumulative, and toxic compounds, and those that determine candidates for future regulation of drinking-water contaminants. The systematic procedures developed and used in this study rely on concepts common to many previously established strategies. The evaluation of pesticide compounds resulted in the classification of compounds into three groups: Tier 1 for high priority compounds, Tier 2 for moderate priority compounds, and Tier 3 for low priority compounds. For water, a total of 247 pesticide compounds were classified as Tier 1 and, thus, are high priority for inclusion in analytical methods for monitoring and studies. Of these, about three-quarters are included in some USGS analytical method; however, many of these compounds are included on research methods that are expensive and for which there are few data on environmental samples. The remaining quarter of Tier 1

  5. Determination of total iodine in serum and urine samples by ion chromatography with pulsed amperometric detection - studies on analyte loss, optimization of sample preparation procedures, and validation of analytical method.

    Science.gov (United States)

    Błażewicz, Anna; Klatka, Maria; Dolliver, Wojciech; Kocjan, Ryszard

    2014-07-01

    A fast, accurate and precise ion chromatography method with pulsed amperometric detection was applied to evaluate a variety of parameters affecting the determination of total iodine in serum and urine of 81 subjects, including 56 obese and 25 healthy Polish children. The sample pretreatment methods were carried out in a closed system and with the assistance of microwaves. Both alkaline and acidic digestion procedures were developed and optimized to find the simplest combination of reagents and the appropriate parameters for digestion that would allow for the fastest, least time consuming and most cost-effective way of analysis. A good correlation between the certified and the measured concentrations was achieved. The best recoveries (96.8% for urine and 98.8% for serum samples) were achieved using 1ml of 25% tetramethylammonium hydroxide solution within 6min for 0.1ml of serum/urine samples. Using 0.5ml of 65% nitric acid solution the best recovery (95.3%) was obtained when 7min of effective digestion time was used. Freeze-thaw stability and long-term stability were checked. After 24 weeks 14.7% loss of iodine in urine, and 10.9% in serum samples occurred. For urine samples, better correlation (R(2)=0.9891) of various sample preparation procedures (alkaline digestion and application of OnGuard RP cartidges) was obtained. Significantly lower iodide content was found in samples taken from obese children. Serum iodine content in obese children was markedly variable in comparison with the healthy group, whereas the difference was less evident when urine samples were analyzed. The mean content in serum was 59.12±8.86μg/L, and in urine 98.26±25.93 for obese children when samples were prepared by the use of optimized alkaline digestion reinforced by microwaves. In healthy children the mean content in serum was 82.58±6.01μg/L, and in urine 145.76±31.44μg/L.

  6. Analytical and computational methods in electromagnetics

    CERN Document Server

    Garg, Ramesh

    2008-01-01

    This authoritative resource offers you clear and complete explanation of this essential electromagnetics knowledge, providing you with the analytical background you need to understand such key approaches as MoM (method of moments), FDTD (Finite Difference Time Domain) and FEM (Finite Element Method), and Green's functions. This comprehensive book includes all math necessary to master the material.

  7. Mathematical methods for physical and analytical chemistry

    CERN Document Server

    Goodson, David Z

    2011-01-01

    Mathematical Methods for Physical and Analytical Chemistry presents mathematical and statistical methods to students of chemistry at the intermediate, post-calculus level. The content includes a review of general calculus; a review of numerical techniques often omitted from calculus courses, such as cubic splines and Newton's method; a detailed treatment of statistical methods for experimental data analysis; complex numbers; extrapolation; linear algebra; and differential equations. With numerous example problems and helpful anecdotes, this text gives chemistry students the mathematical

  8. LC and LC-MS/MS study of forced decomposition behavior of anastrozole and establishment of validated stability-indicating analytical method for impurities estimation in low dose anastrozole tablets.

    Science.gov (United States)

    Reddy, Y Ramachandra; Nandan, Srinivasan R; Bharathi, D Vijaya; Nagaraju, B; Reddy, S Saidu; Ravindranath, L K; Rao, V Suryanarayan

    2009-10-15

    Anastrozole tablets were subjected to different ICH prescribed stress conditions of thermal, hydrolysis, humidity, photolysis and oxidation stress. The drug was found to be stable for all the stressed conditions except for oxidation. Separation of anastrozole from its potential impurities, degradation products and five anastrozole related compounds as main impurities were achieved on Inertsil ODS-3V, 250 mm x 4.6 mm i.d, 5 microm analytical column using reversed phase high performance liquid chromatography (RP-HPLC). The elution of impurities employed time dependent gradient programmed mobile phase consisting of water as mobile phase-A and acetonitrile as mobile phase-B at column flow rates of 1 ml/min and at 215 nm UV detection. The same method was also extended to LC-MS/MS studies which were carried out to identify the degradation product. The method developed was established to have sufficient intermediate precision as similar separation was achieved on another instrument handled by a different operator. The LOQ for anastrozole related compound-A (RC-A), related compound-B (RC-B), related compound-C (RC-C), related compound-D (RC-D), related compound-E (RC-E) and anastrozole were 0.05, 0.03, 0.03, 0.06, 0.06 and 0.06 microg ml(-1) respectively. The linearity of the proposed method for all the above related compounds was investigated in the range of LOQ to 0.600 microg ml(-1) respectively. The specificity was established through peak purity testing using a photo-diode array detector. Method was validated according to ICH guidelines and statistical analysis of the data proved to be suitable for stability testing at quality control.

  9. An inverse and analytic lens design method

    OpenAIRE

    Lu, Yang; Lakshminarayanan, Vasudevan

    2016-01-01

    Traditional lens design is a numerical and forward process based on ray tracing and aberration theory. This method has limitations because the initial configuration of the lens has to be specified and the aberrations of the lenses have to considered. This paper is an initial attempt to investigate an analytic and inverse lens design method, called Lagrange, to overcome these barriers. Lagrange method tries to build differential equations in terms of the system parameters and the system input ...

  10. Towards a full integration of optimization and validation phases: An analytical-quality-by-design approach.

    Science.gov (United States)

    Hubert, C; Houari, S; Rozet, E; Lebrun, P; Hubert, Ph

    2015-05-22

    When using an analytical method, defining an analytical target profile (ATP) focused on quantitative performance represents a key input, and this will drive the method development process. In this context, two case studies were selected in order to demonstrate the potential of a quality-by-design (QbD) strategy when applied to two specific phases of the method lifecycle: the pre-validation study and the validation step. The first case study focused on the improvement of a liquid chromatography (LC) coupled to mass spectrometry (MS) stability-indicating method by the means of the QbD concept. The design of experiments (DoE) conducted during the optimization step (i.e. determination of the qualitative design space (DS)) was performed a posteriori. Additional experiments were performed in order to simultaneously conduct the pre-validation study to assist in defining the DoE to be conducted during the formal validation step. This predicted protocol was compared to the one used during the formal validation. A second case study based on the LC/MS-MS determination of glucosamine and galactosamine in human plasma was considered in order to illustrate an innovative strategy allowing the QbD methodology to be incorporated during the validation phase. An operational space, defined by the qualitative DS, was considered during the validation process rather than a specific set of working conditions as conventionally performed. Results of all the validation parameters conventionally studied were compared to those obtained with this innovative approach for glucosamine and galactosamine. Using this strategy, qualitative and quantitative information were obtained. Consequently, an analyst using this approach would be able to select with great confidence several working conditions within the operational space rather than a given condition for the routine use of the method. This innovative strategy combines both a learning process and a thorough assessment of the risk involved.

  11. Numerical and analytical methods with Matlab

    CERN Document Server

    Bober, William; Masory, Oren

    2013-01-01

    Numerical and Analytical Methods with MATLAB® presents extensive coverage of the MATLAB programming language for engineers. It demonstrates how the built-in functions of MATLAB can be used to solve systems of linear equations, ODEs, roots of transcendental equations, statistical problems, optimization problems, control systems problems, and stress analysis problems. These built-in functions are essentially black boxes to students. By combining MATLAB with basic numerical and analytical techniques, the mystery of what these black boxes might contain is somewhat alleviated. This classroom-tested

  12. Development of quality-by-design analytical methods.

    Science.gov (United States)

    Vogt, Frederick G; Kord, Alireza S

    2011-03-01

    Quality-by-design (QbD) is a systematic approach to drug development, which begins with predefined objectives, and uses science and risk management approaches to gain product and process understanding and ultimately process control. The concept of QbD can be extended to analytical methods. QbD mandates the definition of a goal for the method, and emphasizes thorough evaluation and scouting of alternative methods in a systematic way to obtain optimal method performance. Candidate methods are then carefully assessed in a structured manner for risks, and are challenged to determine if robustness and ruggedness criteria are satisfied. As a result of these studies, the method performance can be understood and improved if necessary, and a control strategy can be defined to manage risk and ensure the method performs as desired when validated and deployed. In this review, the current state of analytical QbD in the industry is detailed with examples of the application of analytical QbD principles to a range of analytical methods, including high-performance liquid chromatography, Karl Fischer titration for moisture content, vibrational spectroscopy for chemical identification, quantitative color measurement, and trace analysis for genotoxic impurities.

  13. Workshop on Analytical Methods in Statistics

    CERN Document Server

    Jurečková, Jana; Maciak, Matúš; Pešta, Michal

    2017-01-01

    This volume collects authoritative contributions on analytical methods and mathematical statistics. The methods presented include resampling techniques; the minimization of divergence; estimation theory and regression, eventually under shape or other constraints or long memory; and iterative approximations when the optimal solution is difficult to achieve. It also investigates probability distributions with respect to their stability, heavy-tailness, Fisher information and other aspects, both asymptotically and non-asymptotically. The book not only presents the latest mathematical and statistical methods and their extensions, but also offers solutions to real-world problems including option pricing. The selected, peer-reviewed contributions were originally presented at the workshop on Analytical Methods in Statistics, AMISTAT 2015, held in Prague, Czech Republic, November 10-13, 2015.

  14. A validated analytical method to study the long-term stability of natural and synthetic glucocorticoids in livestock urine using ultra-high performance liquid chromatography coupled to Orbitrap-high resolution mass spectrometry.

    Science.gov (United States)

    De Clercq, Nathalie; Julie, Vanden Bussche; Croubels, Siska; Delahaut, Philippe; Vanhaecke, Lynn

    2013-08-01

    Due to their growth-promoting effects, the use of synthetic glucocorticoids is strictly regulated in the European Union (Council Directive 2003/74/EC). In the frame of the national control plans, which should ensure the absence of residues in food products of animal origin, in recent years, a higher frequency of prednisolone positive bovine urines has been observed. This has raised questions with respect to the stability of natural corticoids in the respective urine samples and their potential to be transformed into synthetic analogs. In this study, a ultra high performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS) methodology was developed to examine the stability of glucocorticoids in bovine urine under various storage conditions (up to 20 weeks) and to define suitable conditions for sample handling and storage, using an Orbitrap Exactive™. To this end, an extraction procedure was optimized using a Plackett-Burman experimental design to determine the key conditions for optimal extraction of glucocorticoids from urine. Next, the analytical method was successfully validated according to the guidelines of CD 2002/657/EC. Decision limits and detection capabilities for prednisolone, prednisone and methylprednisolone ranged, respectively, from 0.1 to 0.5μgL(-1) and from 0.3 to 0.8μgL(-1). For the natural glucocorticoids limits of detection and limits of quantification for dihydrocortisone, cortisol and cortisone ranged, respectively, from 0.1 to 0.2μgL(-1) and from 0.3 to 0.8μgL(-1). The stability study demonstrated that filter-sterilization of urine, storage at -80°C, and acidic conditions (pH 3) were optimal for preservation of glucocorticoids in urine and able to significantly limit degradation up to 20 weeks.

  15. Algorithmic and analytical methods in network biology.

    Science.gov (United States)

    Koyutürk, Mehmet

    2010-01-01

    During the genomic revolution, algorithmic and analytical methods for organizing, integrating, analyzing, and querying biological sequence data proved invaluable. Today, increasing availability of high-throughput data pertaining to functional states of biomolecules, as well as their interactions, enables genome-scale studies of the cell from a systems perspective. The past decade witnessed significant efforts on the development of computational infrastructure for large-scale modeling and analysis of biological systems, commonly using network models. Such efforts lead to novel insights into the complexity of living systems, through development of sophisticated abstractions, algorithms, and analytical techniques that address a broad range of problems, including the following: (1) inference and reconstruction of complex cellular networks; (2) identification of common and coherent patterns in cellular networks, with a view to understanding the organizing principles and building blocks of cellular signaling, regulation, and metabolism; and (3) characterization of cellular mechanisms that underlie the differences between living systems, in terms of evolutionary diversity, development and differentiation, and complex phenotypes, including human disease. These problems pose significant algorithmic and analytical challenges because of the inherent complexity of the systems being studied; limitations of data in terms of availability, scope, and scale; intractability of resulting computational problems; and limitations of reference models for reliable statistical inference. This article provides a broad overview of existing algorithmic and analytical approaches to these problems, highlights key biological insights provided by these approaches, and outlines emerging opportunities and challenges in computational systems biology.

  16. Wavelet Analytical Forecasting Method of Water Consumption

    Institute of Scientific and Technical Information of China (English)

    刘洪波; 张宏伟

    2004-01-01

    A new method of short-term forecasting for water consumption in municipal supply water networks based on wavelet transformation is introduced. By wavelet decomposing commonly used in the signal field, water consumption per hour is decomposed into many series. Trend item, cycle item and random item are separated from the original time series in this way.Then by analyzing, building a model, forecasting every series and composing the results, the forecasting value of the original consumption is received. Simulation results show that this forecasting method is faster and more accurate, of which the error is less than 20%,indicating that the wavelet analytical method is practicable.

  17. On Analytical Methods in Neuroblastoma Detection

    Directory of Open Access Journals (Sweden)

    R. Martínez-Díaz

    2013-01-01

    quantitative and consistent methods of evaluation are needed to assess reponse to patient therapy. Whole-body I123-metaiodobenzylguanidine (mIBG scintigraphy is used as primary medical image modality to detect neuroblastoma tumours due to its high specificity and sensitivity. However, current oncological guidelines are based on qualitative observer-dependent analysis. This fact makes it difficult to compare results of scintigraphies taken at different moments during therapy or at different institutions. In this paper, we review analytical methods used in neuroblastoma detection and propose an observer-independent method to quantitatively analyse a I123-mIBG scintigraphy.

  18. An analytical method for ditching analysis of an airborne vehicle

    Science.gov (United States)

    Ghaffari, Farhad

    1988-01-01

    A simple analytical method has been introduced for aerohydrodynamic load analysis of an airborne configuration during water ditching. The method employs an aerodynamic panel code, based on linear potential flow theory, to simulate the flow of air and water around an aircraft configuration. The free surface separating the air and water region is represented by doublet sheet singularities. Although all the theoretical load distributions are computed for air, provisions are made to correct the pressure coefficients obtained on the configuration wetted surfaces to account for the water density. As an analytical tool, the Vortex Separation Aerodynamic (VSAERO) code is chosen to carry out the present investigation. After assessing the validity of the method, its first application is to analyze the water ditching of the Space Shuttle configuration at a 12 degree attitude.

  19. Pioglitazone:A review of analytical methods

    Institute of Scientific and Technical Information of China (English)

    N. Satheeshkumar; S. Shantikumar; R. Srinivas

    2014-01-01

    Pioglitazone is an oral anti-hyperglycemic agent. It is used for the treatment of diabetes mellitus type 2. It selectively stimulates nuclear receptor peroxisome proliferator-activated receptor gamma (PPAR-gamma). It was the tenth-best-selling drug in the U.S. in 2008. This article examines published analytical methods reported so far in the literature for the determination of pioglitazone in biological samples and pharmaceutical formulations. They include various techniques like electrochemical methods, spectrophotometry, capillary electrophoresis, high-performance liquid chromatography, liquid chromatography-electrospray ionization-tandem mass spectrometry and high-performance thin layer chromatography.

  20. Directory of Analytical Methods, Department 1820

    Energy Technology Data Exchange (ETDEWEB)

    Whan, R.E. (ed.)

    1986-01-01

    The Materials Characterization Department performs chemical, physical, and thermophysical analyses in support of programs throughout the Laboratories. The department has a wide variety of techniques and instruments staffed by experienced personnel available for these analyses, and we strive to maintain near state-of-the-art technology by continued updates. We have prepared this Directory of Analytical Methods in order to acquaint you with our capabilities and to help you identify personnel who can assist with your analytical needs. The descriptions of the various capabilities are requester-oriented and have been limited in length and detail. Emphasis has been placed on applications and limitations with notations of estimated analysis time and alternative or related techniques. A short, simplified discussion of underlying principles is also presented along with references if more detail is desired. The contents of this document have been organized in the order: bulky analysis, microanalysis, surface analysis, optical and thermal property measurements.

  1. Big data analytics methods and applications

    CERN Document Server

    Rao, BLS; Rao, SB

    2016-01-01

    This book has a collection of articles written by Big Data experts to describe some of the cutting-edge methods and applications from their respective areas of interest, and provides the reader with a detailed overview of the field of Big Data Analytics as it is practiced today. The chapters cover technical aspects of key areas that generate and use Big Data such as management and finance; medicine and healthcare; genome, cytome and microbiome; graphs and networks; Internet of Things; Big Data standards; bench-marking of systems; and others. In addition to different applications, key algorithmic approaches such as graph partitioning, clustering and finite mixture modelling of high-dimensional data are also covered. The varied collection of themes in this volume introduces the reader to the richness of the emerging field of Big Data Analytics.

  2. Modern methods in analytical acoustics lecture notes

    CERN Document Server

    Crighton, D G; Williams, J E Ffowcs; Heckl, M; Leppington, F G

    1992-01-01

    Modern Methods in Analytical Acoustics considers topics fundamental to the understanding of noise, vibration and fluid mechanisms. The series of lectures on which this material is based began by some twenty five years ago and has been developed and expanded ever since. Acknowledged experts in the field have given this course many times in Europe and the USA. Although the scope of the course has widened considerably, the primary aim of teaching analytical techniques of acoustics alongside specific areas of wave motion and unsteady fluid mechanisms remains. The distinguished authors of this volume are drawn from Departments of Acoustics, Engineering of Applied Mathematics in Berlin, Cambridge and London. Their intention is to reach a wider audience of all those concerned with acoustic analysis than has been able to attend the course.

  3. An inverse and analytic lens design method

    CERN Document Server

    Lu, Yang

    2016-01-01

    Traditional lens design is a numerical and forward process based on ray tracing and aberration theory. This method has limitations because the initial configuration of the lens has to be specified and the aberrations of the lenses have to considered. This paper is an initial attempt to investigate an analytic and inverse lens design method, called Lagrange, to overcome these barriers. Lagrange method tries to build differential equations in terms of the system parameters and the system input and output (object and image). The generalized Snell's law in three dimensional space and the normal of a surface in fundamental differential geometry are applied. Based on the Lagrange method equations for a single surface system are derived which can perfectly image a point object.

  4. Fracture mechanics life analytical methods verification testing

    Science.gov (United States)

    Favenesi, J. A.; Clemmons, T. G.; Lambert, T. J.

    1994-01-01

    Verification and validation of the basic information capabilities in NASCRAC has been completed. The basic information includes computation of K versus a, J versus a, and crack opening area versus a. These quantities represent building blocks which NASCRAC uses in its other computations such as fatigue crack life and tearing instability. Several methods were used to verify and validate the basic information capabilities. The simple configurations such as the compact tension specimen and a crack in a finite plate were verified and validated versus handbook solutions for simple loads. For general loads using weight functions, offline integration using standard FORTRAN routines was performed. For more complicated configurations such as corner cracks and semielliptical cracks, NASCRAC solutions were verified and validated versus published results and finite element analyses. A few minor problems were identified in the basic information capabilities of the simple configurations. In the more complicated configurations, significant differences between NASCRAC and reference solutions were observed because NASCRAC calculates its solutions as averaged values across the entire crack front whereas the reference solutions were computed for a single point.

  5. Validación de un método analítico empleando cromatografía líquida de alta eficiencia para la determinación de ibuprofeno en medios biorrelevantes Validation of an analytical method by liquid chromatography for determination of ibuprofen in biorelevant media

    Directory of Open Access Journals (Sweden)

    Sandra M. Gómez

    2010-01-01

    Full Text Available An analytical method by liquid chromatography has been proposed and validated to study the apparent solubility of ibuprofen in biorelevant dissolution media. The main properties of the studied media were pH values of 5.0 and 6.5 and the presence or absence of some natural surfactant agents. The parameters evaluated were specificity, linearity, precision, accuracy, and detection and quantification limits, as well as the drug stability under the analysis conditions. The developed method was useful to determine the apparent solubility of this drug as a function of temperature and surfactants concentration to demonstrate the validity of the Biopharmaceutics Classification System.

  6. Constrained sampling method for analytic continuation

    Science.gov (United States)

    Sandvik, Anders W.

    2016-12-01

    A method for analytic continuation of imaginary-time correlation functions (here obtained in quantum Monte Carlo simulations) to real-frequency spectral functions is proposed. Stochastically sampling a spectrum parametrized by a large number of δ functions, treated as a statistical-mechanics problem, it avoids distortions caused by (as demonstrated here) configurational entropy in previous sampling methods. The key development is the suppression of entropy by constraining the spectral weight to within identifiable optimal bounds and imposing a set number of peaks. As a test case, the dynamic structure factor of the S =1 /2 Heisenberg chain is computed. Very good agreement is found with Bethe ansatz results in the ground state (including a sharp edge) and with exact diagonalization of small systems at elevated temperatures.

  7. Instrumental and Analytic Methods for Bolometric Polarimetry

    CERN Document Server

    Jones, W C; Crill, B P; Contaldi, C R; Kisner, T S; Lange, A E; MacTavish, C J; Netterfield, C B; Ruhl, J E

    2006-01-01

    We discuss instrumental and analytic methods that have been developed for the first generation of bolometric cosmic microwave background (CMB) polarimeters. The design, characterization, and analysis of data obtained using Polarization Sensitive Bolometers (PSBs) are described in detail. This is followed by a brief study of the effect of various polarization modulation techniques on the recovery of sky polarization from scanning polarimeter data. Having been successfully implemented on the sub-orbital Boomerang experiment, PSBs are currently operational in two terrestrial CMB polarization experiments (QUaD and the Robinson Telescope). We investigate two approaches to the analysis of data from these experiments, using realistic simulations of time ordered data to illustrate the impact of instrumental effects on the fidelity of the recovered polarization signal. We find that the analysis of difference time streams takes full advantage of the high degree of common mode rejection afforded by the PSB design. In ad...

  8. The Emergence of the Analytical Method

    DEFF Research Database (Denmark)

    Plum, Maja

    2012-01-01

    Through an analysis of a recent Danish administrative educational reform in the area of early childhood education, this article raises a discussion about the way pedagogical objects and subjects are generated in the knowledge acquisition of administrative educational reforms promoting accountabil...... the nation by an ongoing observational intervention, producing the learning foundation for the entrepreneurial citizen, and thus the nation as a knowledge society in a globalised world. This is what this article terms the emergence of the analytical method....... accountability, visibility and documentation. It is argued that pedagogy is generated as a sequential and unit-specified way of working on the production of ‘the learning child’, forming a time- and material-optimising approach. Hereby, the nursery teacher, as a daily scientific researcher, comes to serve...

  9. Evolution of microbiological analytical methods for dairy industry needs

    Directory of Open Access Journals (Sweden)

    Daniele eSohier

    2014-02-01

    Full Text Available Traditionally, culture-based methods have been used to enumerate microbial populations in dairy products. Recent developments in molecular methods now enable faster and more sensitive analyses than classical microbiology procedures. These molecular tools allow a detailed characterization of cell physiological states and bacterial fitness and thus, offer new perspectives to integration of microbial physiology monitoring to improve industrial processes. This review summarizes the methods described to enumerate and characterize physiological states of technological microbiota in dairy products, and discusses the current deficiencies in relation to the industry’s needs. Recent studies show that PCR-based methods can successfully be applied to quantify fermenting microbes and probiotics in dairy products. Flow cytometry and omics technologies also show interesting analytical potentialities. However, they still suffer from a lack of validation and standardization for quality control analyses, as reflected by the absence of performance studies and official international standards.

  10. 40 CFR 161.180 - Enforcement analytical method.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Enforcement analytical method. 161.180 Section 161.180 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS... § 161.180 Enforcement analytical method. An analytical method suitable for enforcement purposes must...

  11. 40 CFR 158.355 - Enforcement analytical method.

    Science.gov (United States)

    2010-07-01

    ... DATA REQUIREMENTS FOR PESTICIDES Product Chemistry § 158.355 Enforcement analytical method. An analytical method suitable for enforcement purposes must be provided for each active ingredient in the... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Enforcement analytical method....

  12. Microgenetic Learning Analytics Methods: Workshop Report

    Science.gov (United States)

    Aghababyan, Ani; Martin, Taylor; Janisiewicz, Philip; Close, Kevin

    2016-01-01

    Learning analytics is an emerging discipline and, as such, benefits from new tools and methodological approaches. This work reviews and summarizes our workshop on microgenetic data analysis techniques using R, held at the second annual Learning Analytics Summer Institute in Cambridge, Massachusetts, on 30 June 2014. Specifically, this paper…

  13. ANALYTICAL METHODS FOR CALCULATING FAN AERODYNAMICS

    Directory of Open Access Journals (Sweden)

    Jan Dostal

    2015-12-01

    Full Text Available This paper presents results obtained between 2010 and 2014 in the field of fan aerodynamics at the Department of Composite Technology at the VZLÚ aerospace research and experimental institute in Prague – Letnany. The need for rapid and accurate methods for the preliminary design of blade machinery led to the creation of a mathematical model based on the basic laws of turbomachine aerodynamics. The mathematical model, the derivation of which is briefly described below, has been encoded in a computer programme, which enables the theoretical characteristics of a fan of the designed geometry to be determined rapidly. The validity of the mathematical model is assessed continuously by measuring model fans in the measuring unit, which was developed and manufactured specifically for this purpose. The paper also presents a comparison between measured characteristics and characteristics determined by the mathematical model as the basis for a discussion on possible causes of measured deviations and calculation deviations.

  14. Catalyst Kinetics Analytical Method Study of Ruthenium

    Institute of Scientific and Technical Information of China (English)

    Kou ming-ze; Zhan hui-ying; Kou zong-yan

    2004-01-01

    Color reactions are used to determine ruthenium utilizing spectrophotometer, but the process need high temperature, long time pyrogenation and miscellaneous extraction and it contaminates the enviroment. As the sensitive degree and simple apparatus of catalyst kinetics analytical method, it was extensively attentcd. The fundmental principle means to determinn a certain chemistry reaction rate accelerated by homogeneous catalyst and determine substantial content using the function of the numerical value of of its and the catalyst concentration. Color acid double azo-reagents (chloro-phosphor group, arsenic group and carboxylic acid group) are sensitive color reagent determining uranium and thorium of lanthanon, but the report is few that it is used to determine ruthenium. Since 1990s, the author studied that the ruthenium was possessed evident catalysis to the fade reaction of oxidant (KIO4, KBrO3) oxidating color acid double azo-reagent in acitidy medium and provided the catalyst kinetics analytical method to determine trace ruthenium.sensitive degree was increased 1 ~2 amount than color reaction. The reaction as:The original concentration of color acid double azo-reagents is A. The instantaneous absorbency after t reaction time is At. In homogeneous catalyst reaction: log(A0/At) = KCRu3+t. Reaction time t is invarible, so log(A0/At) = K' CRu3+t.Color acid double azo-reagents, such as: chlor-azochlorphosphor(CPA-TC),bromic-azochlorphosphor (CPA-TB), DBS-azochlorphosphor(DBS-CPA), DBC-azochlorphosphor (DBC-CPA), DBOK-azochlorpho sphor (DBOK-CPA), p-iodineazochlorphosphor(CPA-PI),p-acetylazochlorphosphor (CPA-PA), azochlorpho sphorⅢ(CPAⅢ), chlor-azoarsenic (TC-AsA),bromic-azoarsenic (TB-AsA), DBS-azoarsenic(DCS-AsA), DCS-azoarsenic(DCS-AsA),azoarsenicⅢ(AsAⅢ), bromicnityrlazoarsenic (DBN-AsA), P-acetylcarboxy lazo-p,P-acetylcarboxylazo, were utilized in catalyst kinetics system. The author obtains the satisfactory results that color acid double azo-rea gents

  15. Youden test application in robustness assays during method validation.

    Science.gov (United States)

    Karageorgou, Eftichia; Samanidou, Victoria

    2014-08-01

    Analytical method validation is a vital step following method development for ensuring reliable and accurate method performance. Among examined figures of merit, robustness/ruggedness study allows us to test performance characteristics of the analytical process when operating conditions are altered either deliberately or not. This study yields useful information, being a fundamental part of method validation. Since many experiments are required, this step is high demanding in time and consumables. In order to avoid the difficult task of performing too many experiments the Youden test which makes use of fractional factorial designs and has been proved to be a very effective approach. The main advantage of Youden test is the fact that it keeps the required time and effort to a minimum, since only a limited number of determinations have to be made, using combinations of the chosen investigated factors. Typical applications of this robustness test found in literature covering a wide variety of sample matrices are briefly discussed in this review.

  16. Systems and Methods for Composable Analytics

    Science.gov (United States)

    2014-04-29

    runtime, and use the automation server’s application programming interfaces ( APIs ) for creating workspaces, executing commands, and retrieving and setting...with Facebook and Twitter . Users can link their Facebook and Twitter accounts to Composable Analytics using the Oauth protocols, and give Composable...Analytics permission to post on their behalf. We have Facebook and Twitter modules that allow people to automatically publish either text or images

  17. Development and validation of multiresidue analytical method in cotton and groundnut oil for 87 pesticides using low temperature and dispersive cleanup on gas chromatography and liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Chawla, Suchi; Patel, Hemlatta K; Vaghela, Kiran M; Pathan, Firoz Khan; Gor, Hetal N; Patel, Anil R; Shah, Paresh G

    2016-01-01

    A method was developed and validated for the analysis of 87 pesticides in cotton and groundnut oil by GC with ECD and FPD detectors and LC-MS/MS. The extraction procedure based on QuEChERS followed by low-temperature freezing and dispersive cleanup steps was validated in two oil matrices for 87 pesticides of different classes. Linearity, expressed as coefficient of variation, was within the acceptable range. Of those tested, 77-83 and 77-89% pesticides showed recoveries within the acceptable range of 70-120% on LC-MS/MS in cottonseed oil and groundnut oil, respectively, at different spiking levels. In case of GC analysis, 63-65 and 53-82% pesticides showed recoveries within the acceptable range of 70-120% on GC in cottonseed oil and groundnut oil, respectively, at different spiking levels. The exceptions to these recoveries were the few organochlorines which consistently gave lower recoveries. Recovery factors can be employed while analysing these pesticides by this method as the results obtained were consistent in both oils. RSD was less than 20% for most of the pesticides. The calculated limit of quantitation (LOQ) for most of the pesticides satisfies the maximum residue level (MRL) requirements as per European Union (EU) guidelines and Food Safety and Standards Authority of India (FSSAI).

  18. Analytical prediction and field validation of transient temperature field in asphalt pavements

    Institute of Scientific and Technical Information of China (English)

    陈嘉祺; 李亮; 汪浩

    2015-01-01

    This work presented the development and validation of an analytical method to predict the transient temperature field in the asphalt pavement. The governing equation for heat transfer was based on heat conduction radiation and convection. An innovative time-dependent function was proposed to predict the pavement surface temperature with solar radiation and air temperature using dimensional analysis in order to simplify the complex heat exchange on the pavement surface. The parameters for the time-dependent pavement surface temperature function were obtained through the regression analysis of field measurement data. Assuming that the initial pavement temperature distribution was linear and the influence of the base course materials on the temperature of the upper asphalt layers was negligible, a close-form analytical solution of the temperature in asphalt layers was derived using Green’s function. Finally, two numerical examples were presented to validate the model solutions with field temperature measurements. Analysis results show that the solution accuracy is in agreement with field data and the relative errors at a shallower depth are greater than those at a deeper one. Although the model is not sensitive to dramatic changes in climatic factors near the pavement surface, it is applicable for predicting pavement temperature field in cloudless days.

  19. Measuring Students' Writing Ability on a Computer-Analytic Developmental Scale: An Exploratory Validity Study

    Science.gov (United States)

    Burdick, Hal; Swartz, Carl W.; Stenner, A. Jackson; Fitzgerald, Jill; Burdick, Don; Hanlon, Sean T.

    2013-01-01

    The purpose of the study was to explore the validity of a novel computer-analytic developmental scale, the Writing Ability Developmental Scale. On the whole, collective results supported the validity of the scale. It was sensitive to writing ability differences across grades and sensitive to within-grade variability as compared to human-rated…

  20. Numerical-Analytical Method for Magnetic Field Computation in Rotational Electric Machines

    Institute of Scientific and Technical Information of China (English)

    章跃进; 江建中; 屠关镇

    2003-01-01

    A numerical-analytical method is applied for the two-dimensional magnetic field computation in rotational electric machines in this paper. The analytical expressions for air gap magnetic field axe derived. The pole pairs in the expressions are taken into account so that the solution region can be reduced within one periodic range. The numerical and analytical magnetic field equations are linked with equal vector magnetic potential boundary conditions. The magnetic field of a brushless permanent magnet machine is computed by the proposed method. The result is compared to that obtained by finite element method so as to validate the correction of th method.

  1. Fracture mechanics life analytical methods verification testing

    Science.gov (United States)

    Favenesi, J. A.; Clemons, T. G.; Riddell, W. T.; Ingraffea, A. R.; Wawrzynek, P. A.

    1994-01-01

    The objective was to evaluate NASCRAC (trademark) version 2.0, a second generation fracture analysis code, for verification and validity. NASCRAC was evaluated using a combination of comparisons to the literature, closed-form solutions, numerical analyses, and tests. Several limitations and minor errors were detected. Additionally, a number of major flaws were discovered. These major flaws were generally due to application of a specific method or theory, not due to programming logic. Results are presented for the following program capabilities: K versus a, J versus a, crack opening area, life calculation due to fatigue crack growth, tolerable crack size, proof test logic, tearing instability, creep crack growth, crack transitioning, crack retardation due to overloads, and elastic-plastic stress redistribution. It is concluded that the code is an acceptable fracture tool for K solutions of simplified geometries, for a limited number of J and crack opening area solutions, and for fatigue crack propagation with the Paris equation and constant amplitude loads when the Paris equation is applicable.

  2. 清洁效果验证中硫酸卷曲霉素残留量分析方法建立%Establishment of Analytical Method of Capreomycin Sulfate Residual in Cleaning Effect validation

    Institute of Scientific and Technical Information of China (English)

    韦翠; 彭志兴

    2013-01-01

    The cleaning effect of packaging machine needed essential validation in the sterile separation packed process of capreo-mycin sulfate for injection. The residue of the active substance in final rinse water of cleaning validation were determined by HPLC on the column C18 with elution (flow rate: 1.0mL/min), 0.016mol/L hexane sodium solution-methanol-acetonitrile-acetic acid (70∶25∶25∶2,v/v) mixture as mobile phase, UV detection at 254nm. The results showed that suitability, linearity and precision of cleaning validation systemmeet met the analysis demand of the active substance. The method could be applied to the detection of ca-preomycin cleaning effect validation of neomycin residues.%  注射用硫酸卷曲霉素无菌分装过程需要对分装机清洁效果进行验证,本文利用高效液相色谱法对清洁验证最终淋洗水中硫酸卷曲霉素残留量进行检测。色谱条件:以C18色谱柱为固定相,以0.016mol·L-1己烷磺酸钠溶液-甲醇-乙腈-冰醋酸(70∶25∶25∶2,v/v)为流动相,流速为1mL·min-1,紫外检测波长254nm,柱温为常温。结果表明,该方法系统适用性、线性、精密度均符合清洁验证活性物质检测方法要求,可用于清洁效果验证中硫酸卷曲霉素残留量的检测。

  3. An analytic parton shower. Algorithms, implementation and validation

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, Sebastian

    2012-06-15

    The realistic simulation of particle collisions is an indispensable tool to interpret the data measured at high-energy colliders, for example the now running Large Hadron Collider at CERN. These collisions at these colliders are usually simulated in the form of exclusive events. This thesis focuses on the perturbative QCD part involved in the simulation of these events, particularly parton showers and the consistent combination of parton showers and matrix elements. We present an existing parton shower algorithm for emissions off final state partons along with some major improvements. Moreover, we present a new parton shower algorithm for emissions off incoming partons. The aim of these particular algorithms, called analytic parton shower algorithms, is to be able to calculate the probabilities for branchings and for whole events after the event has been generated. This allows a reweighting procedure to be applied after the events have been simulated. We show a detailed description of the algorithms, their implementation and the interfaces to the event generator WHIZARD. Moreover we discuss the implementation of a MLM-type matching procedure and an interface to the shower and hadronization routines from PYTHIA. Finally, we compare several predictions by our implementation to experimental measurements at LEP, Tevatron and LHC, as well as to predictions obtained using PYTHIA. (orig.)

  4. STANDARDIZATION AND VALIDATION OF MICROBIOLOGICAL METHODS FOR EXAMINATION OF BIOSOLIDS

    Science.gov (United States)

    The objective of this presentation is to discuss pathogens of concern in biosolids, the analytical techniques used to evaluate microorganisms in biosolids, and to discuss standardization and validation of analytical protocols for microbes within a complex matrix. Implications of ...

  5. Method for effective usage of Google Analytics tools

    Directory of Open Access Journals (Sweden)

    Ирина Николаевна Егорова

    2016-01-01

    Full Text Available Modern Google Analytics tools have been investigated against effective attraction channels for users and bottlenecks detection. Conducted investigation allowed to suggest modern method for effective usage of Google Analytics tools. The method is based on main traffic indicators analysis, as well as deep analysis of goals and their consecutive tweaking. Method allows to increase website conversion and might be useful for SEO and Web analytics specialists

  6. Rat brain polyamines: an analytical method validation Poliaminas no cérebro do rato: validação de método analítico

    Directory of Open Access Journals (Sweden)

    Valdomiro de Freitas Sampaio

    2010-12-01

    Full Text Available The validation of the analytical technique for the determination of polyamines in cerebral tissue using HPLC based on o-phthalaldehyde post-column derivatization is described. The polyamines were separated in a LiChrospher100 RP18 column. Elution gradient was formed with two mobile phases: A (sodium acetate 0.1 M + sodium octanesulphonate 0.01 M, pH = 4.5 and B (sodium acetate 0.2 M + sodium octanesulphonate 0.01 M/acetonitrile (10:3, pH = 4.5 in a 1.2 ml/min flow rate. The derivative eluent was monitored by fluorescence (excitation, 345 nm; emission, 455 nm. Besides excellent linearity (putrescine, r = 0.9816; spermidine, r = 0.9920; spermine, r = 0.9901, the technique demonstrated intra and inter-day precision (A validação técnica analítica para determinação de poliaminas em tecido cerebral utilizando cromotografia líquida de alta eficiência (HPLC e derivação pós-coluna com o-ftaldialdeído é descrita. A separação das poliaminas deu-se em coluna LiChrospher 100 RP18. O gradiente de eluição foi formado por duas fases móveis A (acetato de sódio 0,1M + octanossulfonato de sódio 0,01 M e B (acetato de sódio 0,2 M + octanossulfonato de sódio 0,01 M/acetonitrila (10:3, fluxo de 1,2 ml/min. O eluente foi monitorado por fluorescência (excitação, 345 nm; emissão, 455 nm. Além da excelente linearidade (putrescina, r = 0,9816; espermidina, r = 0,9920; espermina, r = 0,9901, a técnica demonstrou adequada precisão intra e interdia (< 20% e recuperação (espermidina = 92,56%; espermina = 84,47%. Os limites de quantificação foram 0,22 pM para putrescina, 76,44 pM para espermidina e 51,44 pM para espermina. O método demonstrou ser consistente, simples e altamente reprodutível para a determinação proposta.

  7. Analytic validity of genetic tests to identify factor V Leiden and prothrombin G20210A.

    Science.gov (United States)

    Emadi, Ashkan; Crim, Matthew T; Brotman, Daniel J; Necochea, Alejandro J; Samal, Lipika; Wilson, Lisa M; Bass, Eric B; Segal, Jodi B

    2010-04-01

    The objective of this study is to systematically review methods for detecting Factor V Leiden or prothrombin G20210A. English-language literature from MEDLINE, EMBASE, The Cochrane Library, the Cumulative Index to Nursing and Allied Health Literature, PsycInfo(c), 2000-December 2008. Studies assessed methods for detection of these mutations in at least 10 human blood samples and reported concordance, discordance, or reproducibility. Two investigators abstracted data on the sample selection criteria, test operators, DNA extraction, experimental test, reference standard, commercial instruments, concordance rates, explanation of any discordance, and whether discordance resolved after repetition. We assessed strength of the evidence using the GRADE criteria. We reviewed 7,777 titles and included 66 articles. The majority of the reviewed studies used PCR-RFLP or AS-PCR as the reference standard. The studies demonstrated that commercially available and precommercial tests have high analytic validity with all having greater than 99% concordance with the reference standard. With a few exceptions, discordance resolved with repetition of the test, suggesting operator or administrative errors were responsible for the discordant results. In the quality assurance studies, greater than 98% of laboratories demonstrated high, even perfect, accuracy when asked to diagnose a sample with a known mutation. The majority of errors came from a limited number of laboratories. Although not all methods may be accurate, there is high-grade evidence that genetic tests for the detection of FVL and prothrombin G20210A have excellent analytic validity. There is high-grade evidence that most, but not all, clinical laboratories test for FVL and prothrombin G20210A accurately.

  8. 40 CFR 141.25 - Analytical methods for radioactivity.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 22 2010-07-01 2010-07-01 false Analytical methods for radioactivity... § 141.25 Analytical methods for radioactivity. (a) Analysis for the following contaminants shall be conducted to determine compliance with § 141.66 (radioactivity) in accordance with the methods in...

  9. Nonlinear ordinary differential equations analytical approximation and numerical methods

    CERN Document Server

    Hermann, Martin

    2016-01-01

    The book discusses the solutions to nonlinear ordinary differential equations (ODEs) using analytical and numerical approximation methods. Recently, analytical approximation methods have been largely used in solving linear and nonlinear lower-order ODEs. It also discusses using these methods to solve some strong nonlinear ODEs. There are two chapters devoted to solving nonlinear ODEs using numerical methods, as in practice high-dimensional systems of nonlinear ODEs that cannot be solved by analytical approximate methods are common. Moreover, it studies analytical and numerical techniques for the treatment of parameter-depending ODEs. The book explains various methods for solving nonlinear-oscillator and structural-system problems, including the energy balance method, harmonic balance method, amplitude frequency formulation, variational iteration method, homotopy perturbation method, iteration perturbation method, homotopy analysis method, simple and multiple shooting method, and the nonlinear stabilized march...

  10. Analytical solution methods for geodesic motion

    CERN Document Server

    Hackmann, Eva

    2015-01-01

    The observation of the motion of particles and light near a gravitating object is until now the only way to explore and to measure the gravitational field. In the case of exact black hole solutions of the Einstein equations the gravitational field is characterized by a small number of parameters which can be read off from the observables related to the orbits of test particles and light rays. Here we review the state of the art of analytical solutions of geodesic equations in various space--times. In particular we consider the four dimensional black hole space--times of Pleba\\'nski--Demia\\'nski type as far as the geodesic equation separates, as well as solutions in higher dimensions, and also solutions with cosmic strings. The mathematical tools used are elliptic and hyperelliptic functions. We present a list of analytic solutions which can be found in the literature.

  11. Approximate Analytic and Numerical Solutions to Lane-Emden Equation via Fuzzy Modeling Method

    Directory of Open Access Journals (Sweden)

    De-Gang Wang

    2012-01-01

    Full Text Available A novel algorithm, called variable weight fuzzy marginal linearization (VWFML method, is proposed. This method can supply approximate analytic and numerical solutions to Lane-Emden equations. And it is easy to be implemented and extended for solving other nonlinear differential equations. Numerical examples are included to demonstrate the validity and applicability of the developed technique.

  12. How to assess the quality of your analytical method?

    Science.gov (United States)

    Topic, Elizabeta; Nikolac, Nora; Panteghini, Mauro; Theodorsson, Elvar; Salvagno, Gian Luca; Miler, Marijana; Simundic, Ana-Maria; Infusino, Ilenia; Nordin, Gunnar; Westgard, Sten

    2015-10-01

    Laboratory medicine is amongst the fastest growing fields in medicine, crucial in diagnosis, support of prevention and in the monitoring of disease for individual patients and for the evaluation of treatment for populations of patients. Therefore, high quality and safety in laboratory testing has a prominent role in high-quality healthcare. Applied knowledge and competencies of professionals in laboratory medicine increases the clinical value of laboratory results by decreasing laboratory errors, increasing appropriate utilization of tests, and increasing cost effectiveness. This collective paper provides insights into how to validate the laboratory assays and assess the quality of methods. It is a synopsis of the lectures at the 15th European Federation of Clinical Chemistry and Laboratory Medicine (EFLM) Continuing Postgraduate Course in Clinical Chemistry and Laboratory Medicine entitled "How to assess the quality of your method?" (Zagreb, Croatia, 24-25 October 2015). The leading topics to be discussed include who, what and when to do in validation/verification of methods, verification of imprecision and bias, verification of reference intervals, verification of qualitative test procedures, verification of blood collection systems, comparability of results among methods and analytical systems, limit of detection, limit of quantification and limit of decision, how to assess the measurement uncertainty, the optimal use of Internal Quality Control and External Quality Assessment data, Six Sigma metrics, performance specifications, as well as biological variation. This article, which continues the annual tradition of collective papers from the EFLM continuing postgraduate courses in clinical chemistry and laboratory medicine, aims to provide further contributions by discussing the quality of laboratory methods and measurements and, at the same time, to offer continuing professional development to the attendees.

  13. Analytical methods for heat transfer and fluid flow problems

    CERN Document Server

    Weigand, Bernhard

    2015-01-01

    This book describes useful analytical methods by applying them to real-world problems rather than solving the usual over-simplified classroom problems. The book demonstrates the applicability of analytical methods even for complex problems and guides the reader to a more intuitive understanding of approaches and solutions. Although the solution of Partial Differential Equations by numerical methods is the standard practice in industries, analytical methods are still important for the critical assessment of results derived from advanced computer simulations and the improvement of the underlying numerical techniques. Literature devoted to analytical methods, however, often focuses on theoretical and mathematical aspects and is therefore useless to most engineers. Analytical Methods for Heat Transfer and Fluid Flow Problems addresses engineers and engineering students. The second edition has been updated, the chapters on non-linear problems and on axial heat conduction problems were extended. And worked out exam...

  14. Traveling wave analysis of partial differential equations numerical and analytical methods with Matlab and Maple

    CERN Document Server

    Griffiths, Graham

    2010-01-01

    Although the Partial Differential Equations (PDE) models that are now studied are usually beyond traditional mathematical analysis, the numerical methods that are being developed and used require testing and validation. This is often done with PDEs that have known, exact, analytical solutions. The development of analytical solutions is also an active area of research, with many advances being reported recently, particularly traveling wave solutions for nonlinear evolutionary PDEs. Thus, the current development of analytical solutions directly supports the development of numerical methods by p

  15. Statistically Qualified Neuro-Analytic system and Method for Process Monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Vilim, Richard B.; Garcia, Humberto E.; Chen, Frederick W.

    1998-11-04

    An apparatus and method for monitoring a process involves development and application of a statistically qualified neuro-analytic (SQNA) model to accurately and reliably identify process change. The development of the SQNA model is accomplished in two steps: deterministic model adaption and stochastic model adaptation. Deterministic model adaption involves formulating an analytic model of the process representing known process characteristics,augmenting the analytic model with a neural network that captures unknown process characteristics, and training the resulting neuro-analytic model by adjusting the neural network weights according to a unique scaled equation emor minimization technique. Stochastic model adaptation involves qualifying any remaining uncertainty in the trained neuro-analytic model by formulating a likelihood function, given an error propagation equation, for computing the probability that the neuro-analytic model generates measured process output. Preferably, the developed SQNA model is validated using known sequential probability ratio tests and applied to the process as an on-line monitoring system.

  16. 40 CFR 766.16 - Developing the analytical test method.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Developing the analytical test method... SUBSTANCES CONTROL ACT DIBENZO-PARA-DIOXINS/DIBENZOFURANS General Provisions § 766.16 Developing the analytical test method. Because of the matrix differences of the chemicals listed for testing, no one...

  17. Structural damage localization by outlier analysis of signal-processed mode shapes - Analytical and experimental validation

    Science.gov (United States)

    Ulriksen, M. D.; Damkilde, L.

    2016-02-01

    Contrary to global modal parameters such as eigenfrequencies, mode shapes inherently provide structural information on a local level. Therefore, this particular modal parameter and its derivatives are utilized extensively for damage identification. Typically, more or less advanced mathematical methods are employed to identify damage-induced discontinuities in the spatial mode shape signals, hereby, potentially, facilitating damage detection and/or localization. However, by being based on distinguishing damage-induced discontinuities from other signal irregularities, an intrinsic deficiency in these methods is the high sensitivity towards measurement noise. In the present paper, a damage localization method which, compared to the conventional mode shape-based methods, has greatly enhanced robustness towards measurement noise is proposed. The method is based on signal processing of a spatial mode shape by means of continuous wavelet transformation (CWT) and subsequent application of a generalized discrete Teager-Kaiser energy operator (GDTKEO) to identify damage-induced mode shape discontinuities. In order to evaluate whether the identified discontinuities are in fact damage-induced, outlier analysis is conducted by applying the Mahalanobis metric to major principal scores of the sensor-located bands of the signal-processed mode shape. The method is tested analytically and benchmarked with other mode shape-based damage localization approaches on the basis of a free-vibrating beam and validated experimentally in the context of a residential-sized wind turbine blade subjected to an impulse load.

  18. Experimental validation of structural optimization methods

    Science.gov (United States)

    Adelman, Howard M.

    1992-01-01

    The topic of validating structural optimization methods by use of experimental results is addressed. The need for validating the methods as a way of effecting a greater and an accelerated acceptance of formal optimization methods by practicing engineering designers is described. The range of validation strategies is defined which includes comparison of optimization results with more traditional design approaches, establishing the accuracy of analyses used, and finally experimental validation of the optimization results. Examples of the use of experimental results to validate optimization techniques are described. The examples include experimental validation of the following: optimum design of a trussed beam; combined control-structure design of a cable-supported beam simulating an actively controlled space structure; minimum weight design of a beam with frequency constraints; minimization of the vibration response of helicopter rotor blade; minimum weight design of a turbine blade disk; aeroelastic optimization of an aircraft vertical fin; airfoil shape optimization for drag minimization; optimization of the shape of a hole in a plate for stress minimization; optimization to minimize beam dynamic response; and structural optimization of a low vibration helicopter rotor.

  19. Validity of the nuclear Born-Oppenheimer method

    Energy Technology Data Exchange (ETDEWEB)

    Zettili, N.; Villars, F.M.H.

    1987-07-20

    The validity of the adiabatic nuclear Born-Oppenheimer (NBO) approximation method is investigated by means of an analytically solvable model. The NBO equation of collective motion derived, when this method is applied to the model, is shown to have the structure of a Schroedinger equation. The NBO energy spectrum is then obtained by numerical integration of this equation and compared with the analytic energy spectrum. We show that the NBO approximation is very accurate in the description of the system's eigenstates. The time-dependent Hartree-Fock (TDHF) results, obtained in a previous publication for the solvable model, are compared with their NBO counterparts. We find that, although both methods describe the system's states very well, the NBO approximation is more accurate in the adiabatic domain.

  20. Validity of the nuclear Born-Oppenheimer method

    Science.gov (United States)

    Zettili, Nouredine; Villars, Felix M. H.

    1987-07-01

    The validity of the adiabatic nuclear Born-Oppenheimer (NBO) approximation method is investigated by means of an analytically solvable model. The NBO equation of collective motion derived, when this method is applied to the model, is shown to have the structure of a Schrödinger equation. The NBO energy spectrum is then obtained by numerical integration of this equation and compared with the analytic energy spectrum. We show that the NBO approximation is very accurate in the description of the system's eigenstates. The time-dependent Hartree-Fock (TDHF) results, obtained in a previous publication for the solvable model, are compared with their NBO counterparts. We find that, although both methods describe the system's states very well, the NBO approximation is more accurate in the adiabatic domain.

  1. ASTM Validates Air Pollution Test Methods

    Science.gov (United States)

    Chemical and Engineering News, 1973

    1973-01-01

    The American Society for Testing and Materials (ASTM) has validated six basic methods for measuring pollutants in ambient air as the first part of its Project Threshold. Aim of the project is to establish nationwide consistency in measuring pollutants; determining precision, accuracy and reproducibility of 35 standard measuring methods. (BL)

  2. Some analytical methods for explosives: Part 2

    Energy Technology Data Exchange (ETDEWEB)

    Selig, W.

    1965-12-08

    This report is the second compilation of methods for analyzing explosives. All the methods were developed for routine performance by techniques, and an attempt has therefore been made to keep them as simple as possible. Methods are presented for analyzing plastic-bonded explosives based on sym-cyclomethylenetetra-nitramine (HMX), based on viton in addition to HMX, and based on pentraerythritol tetranitrate (PETN).

  3. Learner Language Analytic Methods and Pedagogical Implications

    Science.gov (United States)

    Dyson, Bronwen

    2010-01-01

    Methods for analysing interlanguage have long aimed to capture learner language in its own right. By surveying the cognitive methods of Error Analysis, Obligatory Occasion Analysis and Frequency Analysis, this paper traces reformulations to attain this goal. The paper then focuses on Emergence Analysis, which fine-tunes learner language analysis…

  4. 7 CFR 94.4 - Analytical methods.

    Science.gov (United States)

    2010-01-01

    ... Association (APHA), the American Water Works Association (AWWA) and the Water Pollution Control Federation, AWWA Bookstore, 6666 West Quincy Avenue, Denver, CO 80235. (h) Test Methods for Evaluating Solid...

  5. Analytical Chemistry: The (Un) Scientific Method.

    Science.gov (United States)

    Laitinen, Herbert A., Ed.

    1979-01-01

    Discusses the proposition that rarely does an investigation follow the orderly and systematic course suggested by the scientific method. The most vital elements are not the experimental and theoretical tools of science, but human ingenuity and intuition. (BT)

  6. 40 CFR 141.704 - Analytical methods.

    Science.gov (United States)

    2010-07-01

    .... (b) E. coli. System must use methods for enumeration of E. coli in source water approved in § 136.3(a... 141.704 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) WATER PROGRAMS (CONTINUED) NATIONAL PRIMARY DRINKING WATER REGULATIONS Enhanced Treatment for Cryptosporidium Source...

  7. Pyrrolizidine alkaloids in honey: comparison of analytical methods

    NARCIS (Netherlands)

    Kempf, M.; Wittig, M.; Reinhard, A.; Ohe, von der K.; Blacquière, T.; Raezke, K.P.; Michel, R.; Schreier, P.; Beuerle, T.

    2011-01-01

    Pyrrolizidine alkaloids (PAs) are a structurally diverse group of toxicologically relevant secondary plant metabolites. Currently, two analytical methods are used to determine PA content in honey. To achieve reasonably high sensitivity and selectivity, mass spectrometry detection is demanded. One me

  8. Analytical chemistry methods for mixed oxide fuel, March 1985

    Energy Technology Data Exchange (ETDEWEB)

    1985-03-01

    This standard provides analytical chemistry methods for the analysis of materials used to produce mixed oxide fuel. These materials are ceramic fuel and insulator pellets and the plutonium and uranium oxides and nitrates used to fabricate these pellets.

  9. Analytical Validation of Accelerator Mass Spectrometry for Pharmaceutical Development: the Measurement of Carbon-14 Isotope Ratio.

    Energy Technology Data Exchange (ETDEWEB)

    Keck, B D; Ognibene, T; Vogel, J S

    2010-02-05

    Accelerator mass spectrometry (AMS) is an isotope based measurement technology that utilizes carbon-14 labeled compounds in the pharmaceutical development process to measure compounds at very low concentrations, empowers microdosing as an investigational tool, and extends the utility of {sup 14}C labeled compounds to dramatically lower levels. It is a form of isotope ratio mass spectrometry that can provide either measurements of total compound equivalents or, when coupled to separation technology such as chromatography, quantitation of specific compounds. The properties of AMS as a measurement technique are investigated here, and the parameters of method validation are shown. AMS, independent of any separation technique to which it may be coupled, is shown to be accurate, linear, precise, and robust. As the sensitivity and universality of AMS is constantly being explored and expanded, this work underpins many areas of pharmaceutical development including drug metabolism as well as absorption, distribution and excretion of pharmaceutical compounds as a fundamental step in drug development. The validation parameters for pharmaceutical analyses were examined for the accelerator mass spectrometry measurement of {sup 14}C/C ratio, independent of chemical separation procedures. The isotope ratio measurement was specific (owing to the {sup 14}C label), stable across samples storage conditions for at least one year, linear over 4 orders of magnitude with an analytical range from one tenth Modern to at least 2000 Modern (instrument specific). Further, accuracy was excellent between 1 and 3 percent while precision expressed as coefficient of variation is between 1 and 6% determined primarily by radiocarbon content and the time spent analyzing a sample. Sensitivity, expressed as LOD and LLOQ was 1 and 10 attomoles of carbon-14 (which can be expressed as compound equivalents) and for a typical small molecule labeled at 10% incorporated with {sup 14}C corresponds to 30 fg

  10. Analytical techniques for instrument design - matrix methods

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, R.A. [Los Alamos National Lab., NM (United States)

    1997-09-01

    We take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalisation to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, we discuss a toolbox of matrix manipulations that can be performed on the 6- dimensional Cooper-Nathans matrix: diagonalisation (Moller-Nielsen method), coordinate changes e.g. from ({Delta}k{sub I},{Delta}k{sub F} to {Delta}E, {Delta}Q & 2 dummy variables), integration of one or more variables (e.g. over such dummy variables), integration subject to linear constraints (e.g. Bragg`s Law for analysers), inversion to give the variance-covariance matrix, and so on. We show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. We will argue that a generalised program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. We will also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question.

  11. Handbook of Analytical Methods for Textile Composites

    Science.gov (United States)

    Cox, Brian N.; Flanagan, Gerry

    1997-01-01

    The purpose of this handbook is to introduce models and computer codes for predicting the properties of textile composites. The handbook includes several models for predicting the stress-strain response all the way to ultimate failure; methods for assessing work of fracture and notch sensitivity; and design rules for avoiding certain critical mechanisms of failure, such as delamination, by proper textile design. The following textiles received some treatment: 2D woven, braided, and knitted/stitched laminates and 3D interlock weaves, and braids.

  12. Analytical techniques for instrument design -- Matrix methods

    Energy Technology Data Exchange (ETDEWEB)

    Robinson, R.A.

    1997-12-31

    The authors take the traditional Cooper-Nathans approach, as has been applied for many years for steady-state triple-axis spectrometers, and consider its generalization to other inelastic scattering spectrometers. This involves a number of simple manipulations of exponentials of quadratic forms. In particular, they discuss a toolbox of matrix manipulations that can be performed on the 6-dimensional Cooper-Nathans matrix. They show how these tools can be combined to solve a number of important problems, within the narrow-band limit and the gaussian approximation. They will argue that a generalized program that can handle multiple different spectrometers could (and should) be written in parallel to the Monte-Carlo packages that are becoming available. They also discuss the complementarity between detailed Monte-Carlo calculations and the approach presented here. In particular, Monte-Carlo methods traditionally simulate the real experiment as performed in practice, given a model scattering law, while the Cooper-Nathans method asks the inverse question: given that a neutron turns up in a particular spectrometer configuration (e.g. angle and time of flight), what is the probability distribution of possible scattering events at the sample? The Monte-Carlo approach could be applied in the same spirit to this question.

  13. Relativistic mirrors in laser plasmas (analytical methods)

    Science.gov (United States)

    Bulanov, S. V.; Esirkepov, T. Zh; Kando, M.; Koga, J.

    2016-10-01

    Relativistic flying mirrors in plasmas are realized as thin dense electron (or electron-ion) layers accelerated by high-intensity electromagnetic waves to velocities close to the speed of light in vacuum. The reflection of an electromagnetic wave from the relativistic mirror results in its energy and frequency changing. In a counter-propagation configuration, the frequency of the reflected wave is multiplied by the factor proportional to the Lorentz factor squared. This scientific area promises the development of sources of ultrashort x-ray pulses in the attosecond range. The expected intensity will reach the level at which the effects predicted by nonlinear quantum electrodynamics start to play a key role. We present an overview of theoretical methods used to describe relativistic flying, accelerating, oscillating mirrors emerging in intense laser-plasma interactions.

  14. A Probabilistic Method for Certification of Analytically Redundant Systems

    Directory of Open Access Journals (Sweden)

    Hu Bin

    2015-03-01

    Full Text Available Analytical fault detection algorithms have the potential to reduce the size, power and weight of safety-critical aerospace systems. Analytical redundancy has been successfully applied in many non-safety critical applications. However, acceptance for aerospace applications will require new methods to rigorously certify the impact of such algorithms on the overall system reliability. This paper presents a theoretical method to assess the probabilistic performance for an analytically redundant system. Specifically, a fault tolerant actuation system is considered. The system consists of dual-redundant actuators and an analytical fault detection algorithm to switch between the hardware components. The exact system failure rate per hour is computed using the law of total probability. This analysis requires knowledge of the failure rates for the hardware components. In addition, knowledge of specific probabilistic performance metrics for the fault detection logic is needed. Numerical examples are provided to demonstrate the proposed analysis method.

  15. An Analytical Method of Auxiliary Sources Solution for Plane Wave Scattering by Impedance Cylinders - A Reference Solution for the Numerical Method of Auxiliary Sources

    DEFF Research Database (Denmark)

    Larsen, Niels Vesterdal; Breinbjerg, Olav

    2004-01-01

    To facilitate the validation of the numerical Method of Auxiliary Sources an analytical Method of Auxiliary Sources solution is derived in this paper. The Analytical solution is valid for transverse magnetic, and electric, plane wave scattering by circular impedance Cylinders, and it is derived...... of the numerical Method of Auxiliary Sources for a range of scattering configurations....... with their singularities at different positions away from the origin. The transformation necessitates a truncation of the wave transformation but the inaccuracy introduced hereby is shown to be negligible. The analytical Method of Auxiliary Sources solution is employed as a reference to investigate the accuracy...

  16. Ethical leadership: meta-analytic evidence of criterion-related and incremental validity.

    Science.gov (United States)

    Ng, Thomas W H; Feldman, Daniel C

    2015-05-01

    This study examines the criterion-related and incremental validity of ethical leadership (EL) with meta-analytic data. Across 101 samples published over the last 15 years (N = 29,620), we observed that EL demonstrated acceptable criterion-related validity with variables that tap followers' job attitudes, job performance, and evaluations of their leaders. Further, followers' trust in the leader mediated the relationships of EL with job attitudes and performance. In terms of incremental validity, we found that EL significantly, albeit weakly in some cases, predicted task performance, citizenship behavior, and counterproductive work behavior-even after controlling for the effects of such variables as transformational leadership, use of contingent rewards, management by exception, interactional fairness, and destructive leadership. The article concludes with a discussion of ways to strengthen the incremental validity of EL. (PsycINFO Database Record

  17. The Validity of Divergent Grounded Theory Method

    Directory of Open Access Journals (Sweden)

    Martin Nils Amsteus PhD

    2014-02-01

    Full Text Available The purpose of this article is to assess whether divergence of grounded theory method may be considered valid. A review of literature provides a basis for understanding and evaluating grounded theory. The principles and nature of grounded theory are synthesized along with theoretical and practical implications. It is deduced that for a theory to be truly grounded in empirical data, the method resulting in the theory should be the equivalent of pure induction. Therefore, detailed, specified, stepwise a priori procedures may be seen as unbidden or arbitrary. It is concluded that divergent grounded theory can be considered valid. The author argues that securing methodological transparency through the description of the actual principles and procedures employed, as well as tailoring them to the particular circumstances, is more important than adhering to predetermined stepwise procedures. A theoretical foundation is provided from which diverse theoretical developments and methodological procedures may be developed, judged, and refined based on their own merits.

  18. Validation of a Serum Analysis Method to Analyze Antihistamines by Capillary Electrophoresis

    Directory of Open Access Journals (Sweden)

    J. Peris-Vicente

    2014-01-01

    Full Text Available The validation of an electrophoresis-based analytical method to quantify 17 antihistamines in pharmaceutical formulations and serum is described. Then, whether the methodology provides true values with low uncertainty and is able to detect the concentration range level of analyte usually found in the matrix was evaluated. The analytical method was validated following the recommendations of an official guide to provide more reliability to the results. The ICH Harmonized Tripartite Guideline was selected because it was especially developed for analysis of drugs. The guide and the following required validation parameters, selectivity, calibration range, linearity, limit of detection, limit of quantification, inter- and intraday accuracy and precision, and robustness, were described. The method was inexpensive, fast, simple, environmentally friendly, and useful for routine analysis. The methodology was successfully validated and applied to commercial pharmaceutical formulations and spiked blank serum samples.

  19. Multicenter validation of the analytical accuracy of Salmonella PCR: towards an international standard

    DEFF Research Database (Denmark)

    Malorny, B.; Hoorfar, Jeffrey; Bunge, C.

    2003-01-01

    Salmonella spp. and 47 non-Salmonella strains. The most selective primer set was found to be 139-141 (K. Rahn, S. A. De Grandis, R. C. Clarke, S. A. McEwen, J. E. Galan, C. Ginocchio, R. Curtiss 111, and C. L. Gyles, Mol. Cell. Probes 6:271-279, 1992), which targets the invA gene. An extended determination...... 16 participating laboratories. Analysis with 28 coded ("blind") DNA samples revealed an analytical accuracy of 98%. Thus, a simple PCR assay that is specific for Salmonella spp. and amplifies a chromosomal DNA fragment detected by gel electrophoresis was established through extensive validation......As part of a major international project for the validation and standardization of PCR for detection of five major food-borne pathogens, four primer sets specific for Salmonella species were evaluated in-house for their analytical accuracy (selectivity and detection limit) in identifying 43...

  20. An AMS method to determine analyte recovery from pharmacokinetic studies with concomitant extravascular and intravenous administration.

    Science.gov (United States)

    Lappin, Graham; Seymour, Mark; Young, Graeme; Higton, David; Hill, Howard M

    2011-02-01

    The absolute bioavailability, clearance and volume of distribution of a drug can be investigated by administering a very low dose of the (14)C-drug intravenously along with a therapeutic nonlabeled dose by the extravascular route (typically orally). The total drug concentration is measured by an assay such as LC-MS and the (14)C-drug is measured by accelerator MS (AMS). In another article in this issue, a method validation is proposed where AMS was used as the analytical assay. Part of the validation is to assess the recovery of the analyte being measured as this has a direct impact on its quantification. In this article, a method of internal standardisation is described where the UV response of the nonlabeled analyte, spiked in excess into the matrix being analysed, is used for internal standardization. The method allows for the recovery of analyte to be measured in each individual sample being analysed. It is important to know the recovery of a (14)C-labeled analyte when determining its mass concentration from (14)C:(12)C isotopic ratio data using AMS. A method is reported in this article that utilizes the UV response of the nonlabeled drug for internal standardization, so that the recovery for each individual sample analyzed can be ascertained.

  1. A Review on Method Development and Validation using HPLC

    Directory of Open Access Journals (Sweden)

    Rashmi Adhikari

    2016-09-01

    Full Text Available High performance liquid chromatography (HPLC is an analytical technique which is used to separate, detect and quantify various drugs and its related degradants. It is employed to separate manufactured drugs from drug related impurities, to detect and quantify synthesized drug and to reduce other impurities at the time of separation. A number of chromatographic parameters were evaluated in order to optimize the method. An appropriate mobile phase, column, column temperature, wavelength and gradient must be found that affords suitable compatibility and stability of drug as well as degradants and impurities. Validation of HPLC as per ICH guidelines covers all the performance characteristics of validation, likeaccuracy, precision, specificity, linearity, range, limit of detection, limit of quantification, robustness and system suitability testing.

  2. Validation of an analytical methodology for the quantitative analysis of petroleum hydrocarbons in marine sediment samples

    Directory of Open Access Journals (Sweden)

    Eloy Yordad Companioni Damas

    2009-01-01

    Full Text Available This work describes a validation of an analytical procedure for the analysis of petroleum hydrocarbons in marine sediment samples. The proposed protocol is able to measure n-alkanes and polycyclic aromatic hydrocarbons (PAH in samples at concentrations as low as 30 ng/g, with a precision better than 15% for most of analytes. The extraction efficiency of fortified sediments varied from 65.1 to 105.6% and 59.7 to 97.8%, for n-alkanes and PAH in the ranges: C16 - C32 and fluoranthene - benzo(apyrene, respectively. The analytical protocol was applied to determine petroleum hydrocarbons in sediments collected from a marine coastal zone.

  3. Recent Advances in Analytical Methods in Mathematical Physics

    OpenAIRE

    Ozer, Teoman; Taranov, Vladimir B.; Smirnov, Roman G.; Klemas, Thomas J.; Thamburaja, Prakash; Wijesinghe, Sanith; Polat, Burak

    2012-01-01

    This special issue of the journal Advances in Mathematical Physics was planned to focus on the most recent advances in analytical techniques of particular use to researchers in the field of mathematical physics that covers a very wide area of topics and has a key role in interdisciplinary studies including mathematics, mechanics, and physics. In this special issue, we were particularly interested in receiving novel contributions detailing analytical methods together with approp...

  4. Fluid dynamics of coarctation of the aorta: analytical solution, in vitro validation and in vivo evaluation

    Science.gov (United States)

    Keshavarz-Motamed, Zahra

    2015-11-01

    Coarctation of the aorta (COA) is a congenital heart disease corresponding to a narrowing in the aorta. Cardiac catheterization is considered to be the reference standard for definitive evaluation of COA severity, based on the peak-to-peak trans-coarctation pressure gradient (PtoP TCPG) and instantaneous systolic value of trans-COA pressure gradient (TCPG). However, invasive cardiac catheterization may carry high risks given that undergoing multiple follow-up cardiac catheterizations in patients with COA is common. The objective of this study is to present an analytical description of the COA that estimates PtoP TCPG and TCPG without a need for high risk invasive data collection. Coupled Navier-Stokes and elastic deformation equations were solved analytically to estimate TCPG and PtoP TCPG. The results were validated against data measured in vitro (e.g., 90% COA: TCPG: root mean squared error (RMSE) = 3.93 mmHg; PtoP TCPG: RMSE = 7.9 mmHg). Moreover, the estimated PtoP TCPG resulted from the suggested analytical description was validated using clinical data in twenty patients with COA (maximum RMSE: 8.3 mmHg). Very good correlation and concordance were found between TCPG and PtoP TCPG obtained from the analytical formulation and in vitro and in vivo data. The suggested methodology can be considered as an alternative to cardiac catheterization and can help preventing its risks.

  5. Development and validation of an analytical method for the separation and determination of major bioactive curcuminoids in Curcuma longa rhizomes and herbal products using non-aqueous capillary electrophoresis.

    Science.gov (United States)

    Anubala, S; Sekar, R; Nagaiah, K

    2014-06-01

    A simple, fast and efficient non-aqueous capillary electrophoresis method (NACE) was developed for the simultaneous determination of three major bioactive curcuminoids (CMNs) in Curcuma longa rhizomes and its herbal products. Good separation, resolution and reproducibility were achieved with the background electrolyte (BGE) consisting a mixture of 15.0 mM sodium tetraborate and 7.4 mM sodium hydroxide (NaOH) in 2:10:15 (v/v/v) of water, 1-propanol, and methanol. The influences of background electrolyte, sodium hydroxide, water, sodium dodecyl sulfate and hydroxylpropyl-β-cyclodextrin on separations were investigated. The separation was carried out in a fused-silica capillary tube with reverse polarity. Hydrodynamic injection of 25mbar for 12s was used for injecting samples and a voltage of 28 kV was applied for separation. The ultrasonication method was used for the extraction of CMNs from the turmeric herbal products and the extract was filtered and directly injected without any further treatments. The limits of detection and quantification were less than 5.0 and 14.6 µg/ml respectively for all CMNs. The percentage recoveries for CMNs were >97.2% (%RSD, <2.62). The results obtained by the method were compared with existing spectrophotometric and HPLC methods. The related compounds in the extract did not interfere in the determination of CMNs. The proposed NACE method is better than existing chromatographic and electrophoretic methods in terms of simple electrophoretic medium, fast analysis and good resolution.

  6. Biological Matrix Effects in Quantitative Tandem Mass Spectrometry-Based Analytical Methods: Advancing Biomonitoring

    Science.gov (United States)

    Panuwet, Parinya; Hunter, Ronald E.; D’Souza, Priya E.; Chen, Xianyu; Radford, Samantha A.; Cohen, Jordan R.; Marder, M. Elizabeth; Kartavenka, Kostya; Ryan, P. Barry; Barr, Dana Boyd

    2015-01-01

    The ability to quantify levels of target analytes in biological samples accurately and precisely, in biomonitoring, involves the use of highly sensitive and selective instrumentation such as tandem mass spectrometers and a thorough understanding of highly variable matrix effects. Typically, matrix effects are caused by co-eluting matrix components that alter the ionization of target analytes as well as the chromatographic response of target analytes, leading to reduced or increased sensitivity of the analysis. Thus, before the desired accuracy and precision standards of laboratory data are achieved, these effects must be characterized and controlled. Here we present our review and observations of matrix effects encountered during the validation and implementation of tandem mass spectrometry-based analytical methods. We also provide systematic, comprehensive laboratory strategies needed to control challenges posed by matrix effects in order to ensure delivery of the most accurate data for biomonitoring studies assessing exposure to environmental toxicants. PMID:25562585

  7. On Approximate Analytical Solutions of Nonlinear Vibrations of Inextensible Beams using Parameter-Expansion Method

    DEFF Research Database (Denmark)

    Kimiaeifar, Amin; Lund, Erik; Thomsen, Ole Thybo;

    2010-01-01

    In this work, an analytical method, which is referred to as Parameter-expansion Method is used to obtain the exact solution for the problem of nonlinear vibrations of an inextensible beam. It is shown that one term in the series expansion is sufficient to obtain a highly accurate solution, which ...... is valid for the whole domain of the problem. A comparison of the obtained the numerical solution demonstrates that PEM is effective and convenient for solving such problems. After validation of the obtained results, the system response and stability are also discussed....

  8. A Process Analytical Technology (PAT) approach to control a new API manufacturing process: development, validation and implementation.

    Science.gov (United States)

    Schaefer, Cédric; Clicq, David; Lecomte, Clémence; Merschaert, Alain; Norrant, Edith; Fotiadu, Frédéric

    2014-03-01

    Pharmaceutical companies are progressively adopting and introducing Process Analytical Technology (PAT) and Quality-by-Design (QbD) concepts promoted by the regulatory agencies, aiming the building of the quality directly into the product by combining thorough scientific understanding and quality risk management. An analytical method based on near infrared (NIR) spectroscopy was developed as a PAT tool to control on-line an API (active pharmaceutical ingredient) manufacturing crystallization step during which the API and residual solvent contents need to be precisely determined to reach the predefined seeding point. An original methodology based on the QbD principles was designed to conduct the development and validation of the NIR method and to ensure that it is fitted for its intended use. On this basis, Partial least squares (PLS) models were developed and optimized using chemometrics methods. The method was fully validated according to the ICH Q2(R1) guideline and using the accuracy profile approach. The dosing ranges were evaluated to 9.0-12.0% w/w for the API and 0.18-1.50% w/w for the residual methanol. As by nature the variability of the sampling method and the reference method are included in the variability obtained for the NIR method during the validation phase, a real-time process monitoring exercise was performed to prove its fit for purpose. The implementation of this in-process control (IPC) method on the industrial plant from the launch of the new API synthesis process will enable automatic control of the final crystallization step in order to ensure a predefined quality level of the API. In addition, several valuable benefits are expected including reduction of the process time, suppression of a rather difficult sampling and tedious off-line analyses.

  9. Analytical and Experimental Modal Analysis for Operational Validation and Calibration of a Miniature Silicon Sensor

    Science.gov (United States)

    Zhang, P. Q.; Tang, X. L.; Shan, B. X.; Brandon, J. A.; Kwan, A. S. K.

    1998-07-01

    The development of micromechanical sensors poses new challenges in design, calibration and operation. The paper reports a study where analytical and experimental techniques are applied to a prototype sensor. Analytically, a substructuring method is used together with a proprietary finite element package. Experimentally, novel excitation and response transducers are used to provide input data for specialised time domain identification algorithms. The resulting comparisons provide confidence in the combination of techniques used in the study.

  10. Validation of Multilevel Constructs: Validation Methods and Empirical Findings for the EDI

    Science.gov (United States)

    Forer, Barry; Zumbo, Bruno D.

    2011-01-01

    The purposes of this paper are to highlight the foundations of multilevel construct validation, describe two methodological approaches and associated analytic techniques, and then apply these approaches and techniques to the multilevel construct validation of a widely-used school readiness measure called the Early Development Instrument (EDI;…

  11. Simplified Analytical Methods to Analyze Lock Gates Submitted to Ship Collisions and Earthquakes

    Directory of Open Access Journals (Sweden)

    Buldgen Loic

    2015-09-01

    Full Text Available This paper presents two simplified analytical methods to analyze lock gates submitted to two different accidental loads. The case of an impact involving a vessel is first investigated. In this situation, the resistance of the struck gate is evaluated by assuming a local and a global deforming mode. The super-element method is used in the first case, while an equivalent beam model is simultaneously introduced to capture the overall bending motion of the structure. The second accidental load considered in this paper is the seismic action, for which an analytical method is presented to evaluate the total hydrodynamic pressure applied on a lock gate during an earthquake, due account being taken of the fluid-structure interaction. For each of these two actions, numerical validations are presented and the analytical results are compared to finite-element solutions.

  12. A Table Lookup Method for Exact Analytical Solutions of Nonlinear Fractional Partial Differential Equations

    Directory of Open Access Journals (Sweden)

    Ji Juan-Juan

    2017-01-01

    Full Text Available A table lookup method for solving nonlinear fractional partial differential equations (fPDEs is proposed in this paper. Looking up the corresponding tables, we can quickly obtain the exact analytical solutions of fPDEs by using this method. To illustrate the validity of the method, we apply it to construct the exact analytical solutions of four nonlinear fPDEs, namely, the time fractional simplified MCH equation, the space-time fractional combined KdV-mKdV equation, the (2+1-dimensional time fractional Zoomeron equation, and the space-time fractional ZKBBM equation. As a result, many new types of exact analytical solutions are obtained including triangular periodic solution, hyperbolic function solution, singular solution, multiple solitary wave solution, and Jacobi elliptic function solution.

  13. A new method for constructing analytic elements for groundwater flow.

    Science.gov (United States)

    Strack, O. D.

    2007-12-01

    The analytic element method is based upon the superposition of analytic functions that are defined throughout the infinite domain, and can be used to meet a variety of boundary conditions. Analytic elements have been use successfully for a number of problems, mainly dealing with the Poisson equation (see, e.g., Theory and Applications of the Analytic Element Method, Reviews of Geophysics, 41,2/1005 2003 by O.D.L. Strack). The majority of these analytic elements consists of functions that exhibit jumps along lines or curves. Such linear analytic elements have been developed also for other partial differential equations, e.g., the modified Helmholz equation and the heat equation, and were constructed by integrating elementary solutions, the point sink and the point doublet, along a line. This approach is limiting for two reasons. First, the existence is required of the elementary solutions, and, second, the integration tends to limit the range of solutions that can be obtained. We present a procedure for generating analytic elements that requires merely the existence of a harmonic function with the desired properties; such functions exist in abundance. The procedure to be presented is used to generalize this harmonic function in such a way that the resulting expression satisfies the applicable differential equation. The approach will be applied, along with numerical examples, for the modified Helmholz equation and for the heat equation, while it is noted that the method is in no way restricted to these equations. The procedure is carried out entirely in terms of complex variables, using Wirtinger calculus.

  14. An Analytical Method for the Abel Inversion of Asymmetrical Gaussian Profiles

    Institute of Scientific and Technical Information of China (English)

    XU Guosheng; WAN Baonian

    2007-01-01

    An analytical algorithm for fast calculation of the Abel inversion for density profile measurement in tokamak is developed. Based upon the assumptions that the particle source is negligibly small in the plasma core region, density profiles can be approximated by an asymmetrical Gaussian distribution controlled only by one parameter V0/D and V0/D is constant along the radial direction, the analytical algorithm is presented and examined against a testing profile. The validity is confirmed by benchmark with the standard Abel inversion method and the theoretical profile. The scope of application as well as the error analysis is also discussed in detail.

  15. Desenvolvimento e validação de um método analítico simples e rápido por espectroscopia UV para quantificação de aciclovir em matrizes hidrofílicas de liberação prolongada Development and validation of a simple and rapid analytical method by UV spectroscopy for acyclovir quantification in hydrophilic matrices for sustained release

    Directory of Open Access Journals (Sweden)

    Fernanda Malaquias Barboza

    2010-01-01

    Full Text Available This work reports the validation of an analytical UV spectrophotometric method to assay acyclovir in hydrophilic matrices (assay and dissolution studies. The method was linear in the range between 2.5-20 µg mL-1, presenting a good correlation coefficient ( r = 0,9999. Precision and accuracy analysis showed low relative standart deviation (< 2.0 % and a good recoveries percentual (98.9-100 %. The procedure was linear, accurate, and robust. The method is simple and cheap. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay acyclovir in hydrophilic matrices tablets.

  16. Literature Review on Processing and Analytical Methods for ...

    Science.gov (United States)

    Report The purpose of this report was to survey the open literature to determine the current state of the science regarding the processing and analytical methods currently available for recovery of F. tularensis from water and soil matrices, and to determine what gaps remain in the collective knowledge concerning F. tularensis identification from environmental samples.

  17. Analytical chemistry methods for metallic core components: Revision March 1985

    Energy Technology Data Exchange (ETDEWEB)

    1985-03-01

    This standard provides analytical chemistry methods for the analysis of alloys used to fabricate core components. These alloys are 302, 308, 316, 316-Ti, and 321 stainless steels and 600 and 718 Inconels and they may include other 300-series stainless steels.

  18. Frontier in nanoscale flows fractional calculus and analytical methods

    CERN Document Server

    Lewis, Roland; Liu, Hong-yan

    2014-01-01

    This ebook covers the basic properties of nanoscale flows, and various analytical and numerical methods for nanoscale flows and environmental flows. This ebook is a good reference not only for audience of the journal, but also for various communities in mathematics, nanotechnology and environmental science.

  19. Decentral gene expression analysis: analytical validation of the Endopredict genomic multianalyte breast cancer prognosis test

    Directory of Open Access Journals (Sweden)

    Kronenwett Ralf

    2012-10-01

    Full Text Available Abstract Background EndoPredict (EP is a clinically validated multianalyte gene expression test to predict distant metastasis in ER-positive, HER2-negative breast cancer treated with endocrine therapy alone. The test is based on the combined analysis of 12 genes in formalin-fixed, paraffin-embedded (FFPE tissue by reverse transcription-quantitative real-time PCR (RT-qPCR. Recently, it was shown that EP is feasible for reliable decentralized assessment of gene expression. The aim of this study was the analytical validation of the performance characteristics of the assay and its verification in a molecular-pathological routine laboratory. Methods Gene expression values to calculate the EP score were assayed by one-step RT-qPCR using RNA from FFPE tumor tissue. Limit of blank, limit of detection, linear range, and PCR efficiency were assessed for each of the 12 PCR assays using serial samples dilutions. Different breast cancer samples were used to evaluate RNA input range, precision and inter-laboratory variability. Results PCR assays were linear up to Cq values between 35.1 and 37.2. Amplification efficiencies ranged from 75% to 101%. The RNA input range without considerable change of the EP score was between 0.16 and 18.5 ng/μl. Analysis of precision (variation of day, day time, instrument, operator, reagent lots resulted in a total noise (standard deviation of 0.16 EP score units on a scale from 0 to 15. The major part of the total noise (SD 0.14 was caused by the replicate-to-replicate noise of the PCR assays (repeatability and was not associated with different operating conditions (reproducibility. Performance characteristics established in the manufacturer’s laboratory were verified in a routine molecular pathology laboratory. Comparison of 10 tumor samples analyzed in two different laboratories showed a Pearson coefficient of 0.995 and a mean deviation of 0.15 score units. Conclusions The EP test showed reproducible performance

  20. Meta-analytic methods for neuroimaging data explained

    Directory of Open Access Journals (Sweden)

    Radua Joaquim

    2012-03-01

    Full Text Available Abstract The number of neuroimaging studies has grown exponentially in recent years and their results are not always consistent. Meta-analyses are helpful to summarize this vast literature and also offer insights that are not apparent from the individual studies. In this review, we describe the main methods used for meta-analyzing neuroimaging data, with special emphasis on their relative advantages and disadvantages. We describe and discuss meta-analytical methods for global brain volumes, methods based on regions of interest, label-based reviews, voxel-based meta-analytic methods and online databases. Regions of interest-based methods allow for optimal statistical analyses but are affected by a limited and potentially biased inclusion of brain regions, whilst voxel-based methods benefit from a more exhaustive and unbiased inclusion of studies but are statistically more limited. There are also relevant differences between the different available voxel-based meta-analytic methods, and the field is rapidly evolving to develop more accurate and robust methods. We suggest that in any meta-analysis of neuroimaging data, authors should aim to: only include studies exploring the whole brain; ensure that the same threshold throughout the whole brain is used within each included study; and explore the robustness of the findings via complementary analyses to minimize the risk of false positives.

  1. A GPU code for analytic continuation through a sampling method

    Science.gov (United States)

    Nordström, Johan; Schött, Johan; Locht, Inka L. M.; Di Marco, Igor

    We here present a code for performing analytic continuation of fermionic Green's functions and self-energies as well as bosonic susceptibilities on a graphics processing unit (GPU). The code is based on the sampling method introduced by Mishchenko et al. (2000), and is written for the widely used CUDA platform from NVidia. Detailed scaling tests are presented, for two different GPUs, in order to highlight the advantages of this code with respect to standard CPU computations. Finally, as an example of possible applications, we provide the analytic continuation of model Gaussian functions, as well as more realistic test cases from many-body physics.

  2. Testing and Validation of the Dynamic Inertia Measurement Method

    Science.gov (United States)

    Chin, Alexander W.; Herrera, Claudia Y.; Spivey, Natalie D.; Fladung, William A.; Cloutier, David

    2015-01-01

    The Dynamic Inertia Measurement (DIM) method uses a ground vibration test setup to determine the mass properties of an object using information from frequency response functions. Most conventional mass properties testing involves using spin tables or pendulum-based swing tests, which for large aerospace vehicles becomes increasingly difficult and time-consuming, and therefore expensive, to perform. The DIM method has been validated on small test articles but has not been successfully proven on large aerospace vehicles. In response, the National Aeronautics and Space Administration Armstrong Flight Research Center (Edwards, California) conducted mass properties testing on an "iron bird" test article that is comparable in mass and scale to a fighter-type aircraft. The simple two-I-beam design of the "iron bird" was selected to ensure accurate analytical mass properties. Traditional swing testing was also performed to compare the level of effort, amount of resources, and quality of data with the DIM method. The DIM test showed favorable results for the center of gravity and moments of inertia; however, the products of inertia showed disagreement with analytical predictions.

  3. O enfoque da metrologia química em análises toxicológicas na atividade turfística: validação de método analítico para determinação de cafeína em matrizes biológicas The chemical metrology approach for toxicological analysis in horseracing: validation of an analytical method for the determination of caffeine in biological matrices

    Directory of Open Access Journals (Sweden)

    India Maria H. de Lima

    2007-01-01

    Full Text Available This paper proposes an alternate method to detect forbidden doping substances present in biological matrices of horseracing. The method was fully validated for caffeine, identified as the most frequent forbidden substance in the analysis conducted by the Antidoping Laboratory of the Brazilian Jockey Club, which adopts a zero threshold limit according to national and international horseracing practices. The metrological reliability of the method applied to toxicological analysis in biological matrices is discussed. Although the analytical method proposed for detection of a zero threshold level of the doping substance is qualitative, it was validated for the determination of the limiting value (also known as quantification limit value introducing a criterion that prevents the issuing of incorrect results ("false-positives" and "false-negatives".

  4. Practical digest for evaluating the uncertainty of analytical assays from validation data according to the LGC/VAM protocol.

    Science.gov (United States)

    González, A Gustavo; Angeles Herrador, M; Asuero, Agustín G

    2005-02-28

    The estimation of the measurement uncertainty of analytical assays based on the LGC/VAM protocol from validation data is fully revisited and discussed in the light of the study of precision, trueness and robustness.

  5. Recent developments in detection methods for microfabricated analytical devices.

    Science.gov (United States)

    Schwarz, M A; Hauser, P C

    2001-09-01

    Sensitive detection in microfluidic analytical devices is a challenge because of the extremely small detection volumes available. Considerable efforts have been made lately to further address this aspect and to investigate techniques other than fluorescence. Among the newly introduced techniques are the optical methods of chemiluminescence, refraction and thermooptics, as well as the electrochemical methods of amperometry, conductimetry and potentiometry. Developments are also in progress to create miniaturized plasma-emission spectrometers and sensitive detectors for gas-chromatographic separations.

  6. Development of Impurity Profiling Methods Using Modern Analytical Techniques.

    Science.gov (United States)

    Ramachandra, Bondigalla

    2017-01-02

    This review gives a brief introduction about the process- and product-related impurities and emphasizes on the development of novel analytical methods for their determination. It describes the application of modern analytical techniques, particularly the ultra-performance liquid chromatography (UPLC), liquid chromatography-mass spectrometry (LC-MS), high-resolution mass spectrometry (HRMS), gas chromatography-mass spectrometry (GC-MS) and high-performance thin layer chromatography (HPTLC). In addition to that, the application of nuclear magnetic resonance (NMR) spectroscopy was also discussed for the characterization of impurities and degradation products. The significance of the quality, efficacy and safety of drug substances/products, including the source of impurities, kinds of impurities, adverse effects by the presence of impurities, quality control of impurities, necessity for the development of impurity profiling methods, identification of impurities and regulatory aspects has been discussed. Other important aspects that have been discussed are forced degradation studies and the development of stability indicating assay methods.

  7. A simple analytical method for deflation prediction of inflatable structures

    Institute of Scientific and Technical Information of China (English)

    李庆松; 卿强; 龚景海

    2015-01-01

    The static performance of inflatable structures has been well studied and the dynamic deployment simulation has received much attention. However, very few studies focus on its deflation behavior. Although there are several dynamic finite element algorithms that can be applied to the deflation simulation, their computation costs are expensive, especially for large scale structures. In this work, a simple method based on classic thermodynamics and the analytical relationship between air and membrane was proposed to efficiently analyze the air state variables under the condition of ventilation. Combined with failure analysis of static bearing capacity, a fast incremental analytical method was presented to predict both elastic and post wrinkling deflation process of inflatable structures. Comparisons between simplified analysis, dynamic finite element simulation, and a full-scale experimental test are presented and the suitability of this simple method for solving the air state and predicting the deflation behavior of inflatable structures is proved.

  8. Modelling of packet traffic with matrix analytic methods

    DEFF Research Database (Denmark)

    Andersen, Allan T.

    1995-01-01

    scenario was modelled using Markovian models. The Ordinary Differential Equations arising from these models were solved numerically. The results obtained seemed very similar to those obtained using a different method in previous work by Akinpelu & Skoog 1985. Recent measurement studies of packet traffic...... process. A heuristic formula for the tail behaviour of a single server queue fed by a superposition of renewal processes has been evaluated. The evaluation was performed by applying Matrix Analytic methods. The heuristic formula has applications in the Call Admission Control (CAC) procedure of the future...... network services i.e. 800 and 900 calls and advanced mobile communication services. The Markovian Arrival Process (MAP) has been used as a versatile tool to model the packet arrival process. Applying the MAP facilitates the use of Matrix Analytic methods to obtain performance measures associated...

  9. Developments and retrospectives in Lie theory geometric and analytic methods

    CERN Document Server

    Penkov, Ivan; Wolf, Joseph

    2014-01-01

    This volume reviews and updates a prominent series of workshops in representation/Lie theory, and reflects the widespread influence of those  workshops in such areas as harmonic analysis, representation theory, differential geometry, algebraic geometry, and mathematical physics.  Many of the contributors have had leading roles in both the classical and modern developments of Lie theory and its applications. This Work, entitled Developments and Retrospectives in Lie Theory, and comprising 26 articles, is organized in two volumes: Algebraic Methods and Geometric and Analytic Methods. This is the Geometric and Analytic Methods volume. The Lie Theory Workshop series, founded by Joe Wolf and Ivan Penkov and joined shortly thereafter by Geoff Mason, has been running for over two decades. Travel to the workshops has usually been supported by the NSF, and local universities have provided hospitality. The workshop talks have been seminal in describing new perspectives in the field covering broad areas of current re...

  10. FORECASTING PILE SETTLEMENT ON CLAYSTONE USING NUMERICAL AND ANALYTICAL METHODS

    Directory of Open Access Journals (Sweden)

    Ponomarev Andrey Budimirovich

    2016-06-01

    Full Text Available In the article the problem of designing pile foundations on claystones is reviewed. The purpose of this paper is comparative analysis of the analytical and numerical methods for forecasting the settlement of piles on claystones. The following tasks were solved during the study: 1 The existing researches of pile settlement are analyzed; 2 The characteristics of experimental studies and the parameters for numerical modeling are presented, methods of field research of single piles’ operation are described; 3 Calculation of single pile settlement is performed using numerical methods in the software package Plaxis 2D and analytical method according to the requirements SP 24.13330.2011; 4 Experimental data is compared with the results of analytical and numerical calculations; 5 Basing on these results recommendations for forecasting pile settlement on claystone are presented. Much attention is paid to the calculation of pile settlement considering the impacted areas in ground space beside pile and the comparison with the results of field experiments. Basing on the obtained results, for the prediction of settlement of single pile on claystone the authors recommend using the analytical method considered in SP 24.13330.2011 with account for the impacted areas in ground space beside driven pile. In the case of forecasting the settlement of single pile on claystone by numerical methods in Plaxis 2D the authors recommend using the Hardening Soil model considering the impacted areas in ground space beside the driven pile. The analyses of the results and calculations are presented for examination and verification; therefore it is necessary to continue the research work of deep foundation at another experimental sites to improve the reliability of the calculation of pile foundation settlement. The work is of great interest for geotechnical engineers engaged in research, design and construction of pile foundations.

  11. A semi-analytical numerical method for fast metamaterial absorber design

    Directory of Open Access Journals (Sweden)

    Y. C. Song

    2015-09-01

    Full Text Available In this paper, a semi-analytical numerical approach utilizing a novel non-grounded model and interpolation technique is introduced to design the frequency selective surface (FSS based metamaterial absorbers (MAs with dramatically reduced time consumption. Different from commonly used trial-and-error technology, our method mainly utilize the numerically computed FSS layer impedance with slow-varying feature in the vicinity of operating frequency. The introduced non-grounded model establishes the quantitative relationship between geometry parameters and equivalent lumped circuit components in conventional transmission line (TL model with reasonable accuracy. The interpolation technique, on the other hand, promises a relative sparse parameter sweep. The detailed design flow as well as analytical explanation with carefully deduced expressions is presented. With the purpose of validating the proposed method and analytical models, a MA with slotted patches is designed through both the semi-analytical numerical approach and the trial-and-error method, where an over 2300 times acceleration is observed. Additionally, results from the analytical computation and full wave simulation agree well with each other.

  12. Validated analytical modeling of diesel engine regulated exhaust CO emission rate

    Directory of Open Access Journals (Sweden)

    Waleed F Faris

    2016-06-01

    Full Text Available Albeit vehicle analytical models are often favorable for explainable mathematical trends, no analytical model has been developed of the regulated diesel exhaust CO emission rate for trucks yet. This research unprecedentedly develops and validates for trucks a model of the steady speed regulated diesel exhaust CO emission rate analytically. It has been found that the steady speed–based CO exhaust emission rate is based on (1 CO2 dissociation, (2 the water–gas shift reaction, and (3 the incomplete combustion of hydrocarbon. It has been found as well that the steady speed–based CO exhaust emission rate based on CO2 dissociation is considerably less than the rate that is based on the water–gas shift reaction. It has also been found that the steady speed–based CO exhaust emission rate based on the water–gas shift reaction is the dominant source of CO exhaust emission. The study shows that the average percentage of deviation of the steady speed–based simulated results from the corresponding field data is 1.7% for all freeway cycles with 99% coefficient of determination at the confidence level of 95%. This deviation of the simulated results from field data outperforms its counterpart of widely recognized models such as the comprehensive modal emissions model and VT-Micro for all freeway cycles.

  13. Development and validation of the analytical method by high performance liquid chromatography (HPLC for Lamotrigine raw material = Desenvolvimento e validação do método analítico por cromatografia líquida de alta eficiência (CLAE para a matéria prima Lamotrigina

    Directory of Open Access Journals (Sweden)

    Guilherme Nobre Lima do Nascimento

    2011-07-01

    Full Text Available Currently when all roads lead to the pursuit of total quality in production of drugs, it is essential to fully understand each phase of a production process. In this case, validation is the appropriate tool to ensure reliability of a production process involving new equipment and the analytical methodology, either in the pharmaceutical, food, computer, microelectronics area or any other area where the quality of the manufactured product is one of the main reasons for the existence of a given company. This study aimed to analyze the main aspects of the validation of analytical methods for Lamotrigine, new drug for bipolar disorder with wide use today. In conclusion, the proposed analytical method for determination of the lamotrigine content in raw materials is adequate, effective and capable of reproducing reliable results during analysis. This method is fast (running time of 10 minutes, selective, accurate, precise and robust for the determination of the drug, with no observedinterfering substances in the optimum wavelength. It could be concluded that this may be a routine method for quality control laboratories to certify the quality of Lamotrigine. Atualmente quando todos os caminhos levam à busca da qualidade total na produção de medicamentos, torna-se indispensável conhecer perfeitamente cada fase de um processo produtivo. Neste caso, a validação é a ferramenta adequada para garantir a confiabilidade de instalação de um processo produtivo, de equipamento novo e, inclusive, da metodologia analítica, seja do setor farmacêutico, alimentício, informática microeletrônico ou qualquer outra área onde a qualidade do produto fabricado é uma das principais razões da existência da empresa. O presente trabalho teve por objetivo analisar os principais aspectos da validação de métodos analíticos para Lamotrigina, fármaco novo para transtorno bipolar com amplo usoatualmente. Em conclusão, o método analítico proposto para determina

  14. Dynamic buckling analysis of delaminated composite plates using semi-analytical finite strip method

    Science.gov (United States)

    Ovesy, H. R.; Totounferoush, A.; Ghannadpour, S. A. M.

    2015-05-01

    The delamination phenomena can become of paramount importance when the design of the composite plates is concerned. In the current study, the effect of through-the-width delamination on dynamic buckling behavior of a composite plate is studied by implementing semi-analytical finite strip method. In this method, the energy and work integrations are computed analytically due to the implementation of trigonometric functions. Moreover, the method can lead to converged results with comparatively small number of degrees of freedom. These features have made the method quite efficient. To account for delamination effects, displacement field is enriched by adding appropriate terms. Also, the penetration of the delamination surfaces is prevented by incorporating an appropriate contact scheme into the time response analysis. Some selected results are validated against those available in the literature.

  15. Comparison between methods of analytical continuation for bosonic functions

    Science.gov (United States)

    Schött, J.; van Loon, E. G. C. P.; Locht, I. L. M.; Katsnelson, M. I.; Di Marco, I.

    2016-12-01

    In this paper we perform a critical assessment of different known methods for the analytical continuation of bosonic functions, namely, the maximum entropy method, the non-negative least-squares method, the non-negative Tikhonov method, the Padé approximant method, and a stochastic sampling method. Four functions of different shape are investigated, corresponding to four physically relevant scenarios. They include a simple two-pole model function; two flavors of the tight-binding model on a square lattice, i.e., a single-orbital metallic system and a two-orbital insulating system; and the Hubbard dimer. The effect of numerical noise in the input data on the analytical continuation is discussed in detail. Overall, the stochastic method by A. S. Mishchenko et al. [Phys. Rev. B 62, 6317 (2000), 10.1103/PhysRevB.62.6317] is shown to be the most reliable tool for input data whose numerical precision is not known. For high-precision input data, this approach is slightly outperformed by the Padé approximant method, which combines a good-resolution power with a good numerical stability. Although none of the methods retrieves all features in the spectra in the presence of noise, our analysis provides a useful guideline for obtaining reliable information of the spectral function in cases of practical interest.

  16. Analytical methods for determination of terbinafine hydrochloride in pharmaceuticals and biological materials$

    Institute of Scientific and Technical Information of China (English)

    Basavaiah Kanakapura n; Vamsi Krishna Penmatsa

    2016-01-01

    Terbinafine is a new powerful antifungal agent indicated for both oral and topical treatment of myco-sessince. It is highly effective in the treatment of determatomycoses. The chemical and pharmaceutical analysis of the drug requires effective analytical methods for quality control and pharmacodynamic and pharmacokinetic studies. Ever since it was introduced as an effective antifungal agent, many methods have been developed and validated for its assay in pharmaceuticals and biological materials. This article reviews the various methods reported during the last 25 years.

  17. Analytical method for determination of benzene-arsenic acids

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, G.L.; Bayse, G.S.

    1988-01-01

    A sensitive analytical method has been modified for use in determination of several benzenearsonic acids, including arsanilic acid (p-aminobenzenearsonic acid), Roxarsone (3-nitro-4-hydroxybenzenearsonic acid), and p-ureidobenzene arsonic acid. Controlled acid hydrolysis of these compounds produces a quantitative yield of arsenate, which is measured colorimetrically as the molybdenum blue complex at 865 nm. The method obeys Beer's Law over the micromolar concentration range. These benzenearsonic acids are routinely used as feed additives in poultry and swine. This method should be useful in assessing tissue levels of the arsenicals in appropriate extracts.

  18. Customizing computational methods for visual analytics with big data.

    Science.gov (United States)

    Choo, Jaegul; Park, Haesun

    2013-01-01

    The volume of available data has been growing exponentially, increasing data problem's complexity and obscurity. In response, visual analytics (VA) has gained attention, yet its solutions haven't scaled well for big data. Computational methods can improve VA's scalability by giving users compact, meaningful information about the input data. However, the significant computation time these methods require hinders real-time interactive visualization of big data. By addressing crucial discrepancies between these methods and VA regarding precision and convergence, researchers have proposed ways to customize them for VA. These approaches, which include low-precision computation and iteration-level interactive visualization, ensure real-time interactive VA for big data.

  19. Toward a Unified Validation Framework in Mixed Methods Research

    Science.gov (United States)

    Dellinger, Amy B.; Leech, Nancy L.

    2007-01-01

    The primary purpose of this article is to further discussions of validity in mixed methods research by introducing a validation framework to guide thinking about validity in this area. To justify the use of this framework, the authors discuss traditional terminology and validity criteria for quantitative and qualitative research, as well as…

  20. Simplified Analytical Method for Optimized Initial Shape Analysis of Self-Anchored Suspension Bridges and Its Verification

    Directory of Open Access Journals (Sweden)

    Myung-Rag Jung

    2015-01-01

    Full Text Available A simplified analytical method providing accurate unstrained lengths of all structural elements is proposed to find the optimized initial state of self-anchored suspension bridges under dead loads. For this, equilibrium equations of the main girder and the main cable system are derived and solved by evaluating the self-weights of cable members using unstrained cable lengths and iteratively updating both the horizontal tension component and the vertical profile of the main cable. Furthermore, to demonstrate the validity of the simplified analytical method, the unstrained element length method (ULM is applied to suspension bridge models based on the unstressed lengths of both cable and frame members calculated from the analytical method. Through numerical examples, it is demonstrated that the proposed analytical method can indeed provide an optimized initial solution by showing that both the simplified method and the nonlinear FE procedure lead to practically identical initial configurations with only localized small bending moment distributions.

  1. The moment propagation method for advection-diffusion in the lattice Boltzmann method: validation and Péclet number limits

    NARCIS (Netherlands)

    Merks, R.M.H.; Hoekstra, A.G.; Sloot, P.M.A.

    2002-01-01

    We numerically validate the moment propagation method for advection-diffusion in a Lattice Boltzmann simulation against the analytic Taylor-Aris prediction for dispeion in a three dimensional Poiseuille flow. Good agreement between simulation and teh tehory is found, with relative errors smaller tha

  2. An analytical method for the ditching analysis of an airborne vehicle

    Science.gov (United States)

    Ghaffari, Farhad

    1988-01-01

    A simple analytical method has been introduced for aerohydrodynamic load analysis of an airborne configuration during water ditching. The method employs an aerodynamic panel code, based on linear potential flow theory, to simulate the flow of air and water around an aircraft configuration. The free surface separating the air and water region is represented by doublet sheet singularities. Although all the theoretical load distributions are computed for air, provisions are made to correct the pressure coefficients obtained on the configuration wetted surfaces to account for the water density. As an analytical tool, the Vortex Separation Aerodynamic (VSAERO) code is chosen to carry out the present investigation. After assessing the validity of the method, its first application is to analyze the water ditching of the Space Shuttle configuration at a 12 degree attitude.

  3. Methods for developing and validating survivability distributions

    Energy Technology Data Exchange (ETDEWEB)

    Williams, R.L.

    1993-10-01

    A previous report explored and discussed statistical methods and procedures that may be applied to validate the survivability of a complex system of systems that cannot be tested as an entity. It described a methodology where Monte Carlo simulation was used to develop the system survivability distribution from the component distributions using a system model that registers the logical interactions of the components to perform system functions. This paper discusses methods that can be used to develop the required survivability distributions based upon three sources of knowledge. These are (1) available test results; (2) little or no available test data, but a good understanding of the physical laws and phenomena which can be applied by computer simulation; and (3) neither test data nor adequate knowledge of the physics are known, in which case, one must rely upon, and quantify, the judgement of experts. This paper describes the relationship between the confidence bounds that can be placed on survivability and the number of tests conducted. It discusses the procedure for developing system level survivability distributions from the distributions for lower levels of integration. It demonstrates application of these techniques by defining a communications network for a Hypothetical System Architecture. A logic model for the performance of this communications network is developed, as well as the survivability distributions for the nodes and links based on two alternate data sets, reflecting the effects of increased testing of all elements. It then shows how this additional testing could be optimized by concentrating only on those elements contained in the low-order fault sets which the methodology identifies.

  4. Benchmark Comparison of Cloud Analytics Methods Applied to Earth Observations

    Science.gov (United States)

    Lynnes, Chris; Little, Mike; Huang, Thomas; Jacob, Joseph; Yang, Phil; Kuo, Kwo-Sen

    2016-01-01

    Cloud computing has the potential to bring high performance computing capabilities to the average science researcher. However, in order to take full advantage of cloud capabilities, the science data used in the analysis must often be reorganized. This typically involves sharding the data across multiple nodes to enable relatively fine-grained parallelism. This can be either via cloud-based file systems or cloud-enabled databases such as Cassandra, Rasdaman or SciDB. Since storing an extra copy of data leads to increased cost and data management complexity, NASA is interested in determining the benefits and costs of various cloud analytics methods for real Earth Observation cases. Accordingly, NASA's Earth Science Technology Office and Earth Science Data and Information Systems project have teamed with cloud analytics practitioners to run a benchmark comparison on cloud analytics methods using the same input data and analysis algorithms. We have particularly looked at analysis algorithms that work over long time series, because these are particularly intractable for many Earth Observation datasets which typically store data with one or just a few time steps per file. This post will present side-by-side cost and performance results for several common Earth observation analysis operations.

  5. SRXRF Experiments and Analytical Methods of Mineral Individual Fluid Inclusions

    Institute of Scientific and Technical Information of China (English)

    Wu Chunxue; Huang Yuying; Li Hongkui; Chen Chuanren; He Wei; Li Kuifa

    2007-01-01

    This paper focuses on the micro-beam and trace element non-destructive experiment and analytical method of mineral fluid inclusions by synchrotron radiation X-ray fluorescence (SRXRF) microprobe at Beijing Synchrotron Radiation Facility (BSRF). The experimental instrument, measurement process and calculating method are introduced. A set of oil- and gas-containing typical mineral fluid inclusions taken from the Tazhong and Lunnan oilfields in the Tarim Basin were analyzed non-destructively. The trace element contents in the fluid inclusions may provide guidance for oil and gas exploration and development.

  6. Analytical methods used to measure acrylamide concentrations in foods.

    Science.gov (United States)

    Castle, Laurence; Eriksson, Sune

    2005-01-01

    The state-of-the-art of analysis for acrylamide in food is reviewed. The majority of analytical methods adopts a similar approach: addition of internal standard to the specimen, extraction with water, purification of extract using a solid-phase extraction cartridge, and then determination using either gas chromatography coupled to mass spectroscopy (GC/MS) after bromination, or direct measurement with liquid chromatography coupled to mass spectroscopy (LC/MS). The available methods generally show good agreement and are likely to be accurate. However, improvements in precision (within-laboratory) and repeatability (between-laboratory) are needed by particular data users.

  7. Standardization of chemical analytical techniques for pyrolysis bio-oil: history, challenges, and current status of methods: Bio-oil Analytical Standardization

    Energy Technology Data Exchange (ETDEWEB)

    Ferrell, Jack R. [National Renewable Energy Laboratory (NREL), Golden CO USA; Olarte, Mariefel V. [Pacific Northwest National Laboratory (PNNL), Richland WA USA; Christensen, Earl D. [National Renewable Energy Laboratory (NREL), Golden CO USA; Padmaperuma, Asanga B. [Pacific Northwest National Laboratory (PNNL), Richland WA USA; Connatser, Raynella M. [Oak Ridge National Laboratory (ORNL), Oak Ridge TN USA; Stankovikj, Filip [Washington State University (WSU), Pullman WA USA; Meier, Dietrich [Thünen Institute of Wood Research (TI), Hamburg Germany; Paasikallio, Ville [VTT Technical Research Centre of Finland Ltd (VTT), Espoo Finland

    2016-07-05

    In this perspective, we discuss the standardization of analytical techniques for pyrolysis bio-oils, including the current status of methods, and our opinions on future directions. First, the history of past standardization efforts is summarized, and both successful and unsuccessful validation of analytical techniques highlighted. The majority of analytical standardization studies to-date has tested only physical characterization techniques. Here, we present results from an international round robin on the validation of chemical characterization techniques for bio-oils. Techniques tested included acid number, carbonyl titrations using two different methods (one at room temperature and one at 80 degrees C), 31P NMR for determination of hydroxyl groups, and a quantitative gas chromatography-mass spectrometry (GC-MS) method. Both carbonyl titration and acid number methods have yielded acceptable inter-laboratory variabilities. 31P NMR produced acceptable results for aliphatic and phenolic hydroxyl groups, but not for carboxylic hydroxyl groups. As shown in previous round robins, GC-MS results were more variable. Reliable chemical characterization of bio-oils will enable upgrading research and allow for detailed comparisons of bio-oils produced at different facilities. Reliable analytics are also needed to enable an emerging bioenergy industry, as processing facilities often have different analytical needs and capabilities than research facilities. We feel that correlations in reliable characterizations of bio-oils will help strike a balance between research and industry, and will ultimately help to determine metrics for bio-oil quality. Finally, the standardization of additional analytical methods is needed, particularly for upgraded bio-oils.

  8. The Method of Manufactured Universes for validating uncertainty quantification methods

    KAUST Repository

    Stripling, H.F.

    2011-09-01

    The Method of Manufactured Universes is presented as a validation framework for uncertainty quantification (UQ) methodologies and as a tool for exploring the effects of statistical and modeling assumptions embedded in these methods. The framework calls for a manufactured reality from which experimental data are created (possibly with experimental error), an imperfect model (with uncertain inputs) from which simulation results are created (possibly with numerical error), the application of a system for quantifying uncertainties in model predictions, and an assessment of how accurately those uncertainties are quantified. The application presented in this paper manufactures a particle-transport universe, models it using diffusion theory with uncertain material parameters, and applies both Gaussian process and Bayesian MARS algorithms to make quantitative predictions about new experiments within the manufactured reality. The results of this preliminary study indicate that, even in a simple problem, the improper application of a specific UQ method or unrealized effects of a modeling assumption may produce inaccurate predictions. We conclude that the validation framework presented in this paper is a powerful and flexible tool for the investigation and understanding of UQ methodologies. © 2011 Elsevier Ltd. All rights reserved.

  9. Validation of methods for the detection and quantification of engineered nanoparticles in food

    DEFF Research Database (Denmark)

    Linsinger, T.P.J.; Chaudhry, Q.; Dehalu, V.

    2013-01-01

    The potential impact of nanomaterials on the environment and on human health has already triggered legislation requiring labelling of products containing nanoparticles. However, so far, no validated analytical methods for the implementation of this legislation exist. This paper outlines a generic...

  10. An Analytical Method for Positioning Drag Anchors in Seabed Soils

    Institute of Scientific and Technical Information of China (English)

    张炜; 刘海笑; 李新仲; 李清平; 曹静

    2015-01-01

    Positioning drag anchors in seabed soils are strongly influenced not only by the properties of the anchor and soil, but also by the characteristics of the installation line. The investigation on the previous prediction methods related to anchor positioning demonstrates that the prediction of the anchor position during dragging has inevitably introduced some key and unsubstantiated hypotheses and the applicability of these methods is limited. In the present study, the interactional system between the drag anchor and installation line is firstly introduced for the analysis of anchor positioning. Based on the two mechanical models for embedded lines and drag anchors, the positioning equations for drag anchors have been derived both for cohesive and noncohesive soils. Since the drag angle at the shackle is the most important parameter in the positioning equations, a novel analytical method that can predict both the variation and the exact value of the drag angle at the shackle is proposed. The analytical method for positioning drag anchors which combines the interactional system between the drag anchor and the installation line has provided a reasonable theoretic approach to investigate the anchor behaviors in soils. By comparing with the model flume experiments, the sensitivity, effectiveness and veracity of the positioning method are well verified.

  11. Comparison of analytical methods for calculation of wind loads

    Science.gov (United States)

    Minderman, Donald J.; Schultz, Larry L.

    1989-01-01

    The following analysis is a comparison of analytical methods for calculation of wind load pressures. The analytical methods specified in ASCE Paper No. 3269, ANSI A58.1-1982, the Standard Building Code, and the Uniform Building Code were analyzed using various hurricane speeds to determine the differences in the calculated results. The winds used for the analysis ranged from 100 mph to 125 mph and applied inland from the shoreline of a large open body of water (i.e., an enormous lake or the ocean) a distance of 1500 feet or ten times the height of the building or structure considered. For a building or structure less than or equal to 250 feet in height acted upon by a wind greater than or equal to 115 mph, it was determined that the method specified in ANSI A58.1-1982 calculates a larger wind load pressure than the other methods. For a building or structure between 250 feet and 500 feet tall acted upon by a wind rangind from 100 mph to 110 mph, there is no clear choice of which method to use; for these cases, factors that must be considered are the steady-state or peak wind velocity, the geographic location, the distance from a large open body of water, and the expected design life and its risk factor.

  12. An Analytic Method for Measuring Accurate Fundamental Frequency Components

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Soon Ryul; Park Jong Keun [Seoul National University, Seoul(Korea); Kang, Sang Hee [Myongji University, Seoul (Korea)

    2002-04-01

    This paper proposes an analytic method for measuring the accurate fundamental frequency component of a fault current signal distorted with a DC-offset, a characteristic frequency component, and harmonics. The proposed algorithm is composed of four stages: sine filer, linear filter, Prony's method, and measurement. The sine filter and the linear filter eliminate harmonics and the fundamental frequency component, respectively. Then Prony's method is used to estimate the parameters of the DC-offset and the characteristic frequency component. Finally, the fundamental frequency component is measured by compensating the sine-filtered signal with the estimated parameters. The performance evaluation of the proposed method is presented for a-phase to ground faults on a 345 kV 200 km overhead transmission line. The EMTP is used to generate fault current signals under different fault locations and fault inception angles. It is shown that the analytic method accurately measures the fundamental frequency component regardless of the characteristic frequency component as well as the DC-offset.(author). 19 refs., 4 figs., 4 tabs.

  13. Toward a quality guide to facilitate the transference of analytical methods from research to testing laboratories: a case study.

    Science.gov (United States)

    Bisetty, Krisnha; Gumede, Njabulo Joyfull; Escuder-Gilabert, Laura; Sagrado, Salvador

    2009-01-01

    At present, there is no single viewpoint that defines QA strategies in analytical chemistry. On the other hand, there are no unique protocols defining a set of analytical tasks and decision criteria to be performed during the method development phase (e.g., by a single research laboratory) in order to facilitate the transference to the testing laboratories intending to adapt, validate, and routinely use this method. This study proposes general criteria, a priori valid for any developed method, recommended as a provisional quality guide containing the minimum internal tasks necessary to publish new analytical method results. As an application, the selection of some basic internal quality tasks and the corresponding accepted criteria are adapted to a concrete case study: indirect differential pulse polarographic determination of nitrate in water samples according to European Commission requisites. Extra tasks to be performed by testing laboratories are also outlined.

  14. Analytical validation of the Roche 25-OH Vitamin D Total assay

    DEFF Research Database (Denmark)

    Knudsen, Cindy Soendersoe; Nexo, Ebba; Højskov, Carsten Schriver;

    2012-01-01

    Background: Vitamin D deficiency is considered a major health issue and therefore there is a need for reliable routine tests for measurement of the vitamin in blood samples. Here we present a validation of the recently released Roche 25-OH Vitamin D Total assay (Vitamin D Total). Methods: We anal...

  15. Method for sensing an analyte in a fluid and sensor unit for such method

    NARCIS (Netherlands)

    Dekker, N.H.; Pedaci, F.; Barland, S.

    2012-01-01

    The invention provides a method for sensing with a sensor system an analyte in an analyte fluid. The sensor system comprises a micron scale birefringent entity, a laser unit configured to generate polarized laser light, a polarization rotation device, wherein the laser unit and polarization rotation

  16. A Validated Analytical Model for Availability Prediction of IPTV Services in VANETs

    Directory of Open Access Journals (Sweden)

    Bernd E. Wolfinger

    2014-12-01

    Full Text Available In vehicular ad hoc networks (VANETs, besides the original applications typically related to traffic safety, we nowadays can observe an increasing trend toward infotainment applications, such as IPTV services. Quality of experience (QoE, as observed by the end users of IPTV, is highly important to guarantee adequate user acceptance for the service. In IPTV, QoE is mainly determined by the availability of TV channels for the users. This paper presents an efficient and rather generally applicable analytical model that allows one to predict the blocking probability of TV channels, both for channel-switching-induced, as well as for handover-induced blocking events. We present the successful validation of the model by means of simulation, and we introduce a new measure for QoE. Numerous case studies illustrate how the analytical model and our new QoE measure can be applied successfully for the dimensioning of IPTV systems, taking into account the QoE requirements of the IPTV service users in strongly diverse traffic scenarios.

  17. Effective method for calculation of the analytic QCD coupling constant

    CERN Document Server

    Alekseev, A Yu

    2002-01-01

    The analytic running coupling of strong interaction alpha sub a sub n for initial standard perturbative approximations up to three-loop order is studied. The nonperturbative contributions to alpha sub a sub n are obtained in an explicit form. They are shown to be represented in the form of the expansion in the inverse powers of Euclidean momentum squared. It is shown that two-loop and three-loop-order corrections result in partial compensation of one-loop-order leading in the ultraviolet region nonperturbative contribution of the form 1/q sup 2. On basis of the stated expansion the effective method for calculation of the analytic running coupling is developed for all q > LAMBDA. The comparative analysis of the perturbative and nonperturbative contributions is carried out in the momentum dependence of alpha sub a sub n and its perturbative component for one - three-loop cases leads to a conclusion on higher loop stability of the analytic running coupling and its low dependence on the n sub f -threshold matchin...

  18. Selectivity in analytical chemistry: two interpretations for univariate methods.

    Science.gov (United States)

    Dorkó, Zsanett; Verbić, Tatjana; Horvai, George

    2015-01-01

    Selectivity is extremely important in analytical chemistry but its definition is elusive despite continued efforts by professional organizations and individual scientists. This paper shows that the existing selectivity concepts for univariate analytical methods broadly fall in two classes: selectivity concepts based on measurement error and concepts based on response surfaces (the response surface being the 3D plot of the univariate signal as a function of analyte and interferent concentration, respectively). The strengths and weaknesses of the different definitions are analyzed and contradictions between them unveiled. The error based selectivity is very general and very safe but its application to a range of samples (as opposed to a single sample) requires the knowledge of some constraint about the possible sample compositions. The selectivity concepts based on the response surface are easily applied to linear response surfaces but may lead to difficulties and counterintuitive results when applied to nonlinear response surfaces. A particular advantage of this class of selectivity is that with linear response surfaces it can provide a concentration independent measure of selectivity. In contrast, the error based selectivity concept allows only yes/no type decision about selectivity.

  19. Comparison of analytical methods for HULIS measurements in atmospheric particles

    Directory of Open Access Journals (Sweden)

    C. Baduel

    2009-03-01

    Full Text Available Humic-Like Substances (HULIS are a major contributor to the organic carbon in atmospheric aerosol. It would be necessary to standardise an analytical method that could be easily and routinely used for HULIS measurements. We present one of the first comparisons of two of the main methods in use to extract HULIS, using i a weak anion exchanger (DEAE and ii the combination of two separation steps, one according to polarity (on C18 and the second according to acidity (with a strong anion exchanger SAX. The quantification is performed with a DOC analyzer, complemented by an investigation of the chemical structure of the extracted fractions by UV-Visible spectroscopy. The analytical performances of each method are determined and compared for humic substances standards. These methods are further applied to determine the water extractable HULIS (HULISWS and the 0.1M NaOH alkaline extractable HULIS (HULIST in atmospheric aerosol collected in an Alpine Valley during winter time. This comparison shows that the simpler DEAE isolation procedure leads to higher recoveries and better reproducibility and should therefore be recommended.

  20. Gaussian Analytic Centroiding method of star image of star tracker

    Science.gov (United States)

    Wang, Haiyong; Xu, Ershuai; Li, Zhifeng; Li, Jingjin; Qin, Tianmu

    2015-11-01

    The energy distribution of an actual star image coincides with the Gaussian law statistically in most cases, so the optimized processing algorithm about star image centroiding should be constructed also by following Gaussian law. For a star image spot covering a certain number of pixels, the marginal distribution of the gray accumulation on rows and columns are shown and analyzed, based on which the formulas of Gaussian Analytic Centroiding method (GAC) are deduced, and the robustness is also promoted due to the inherited filtering effect of gray accumulation. Ideal reference star images are simulated by the PSF (point spread function) with integral form. Precision and speed tests for the Gaussian Analytic formulas are conducted under three scenarios of Gaussian radius (0.5, 0.671, 0.8 pixel), The simulation results show that the precision of GAC method is better than that of the other given algorithms when the Gaussian radius is not bigger than 5 × 5 pixel window, a widely used parameter. Above all, the algorithm which consumes the least time is still the novel GAC method. GAC method helps to promote the comprehensive performance in the attitude determination of a star tracker.

  1. A nonlinear analytic function expansion nodal method for transient calculations

    Energy Technology Data Exchange (ETDEWEB)

    Joo, Han Gyn; Park, Sang Yoon; Cho, Byung Oh; Zee, Sung Quun [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1998-12-31

    The nonlinear analytic function expansion nodal (AFEN) method is applied to the solution of the time-dependent neutron diffusion equation. Since the AFEN method requires both the particular solution and the homogeneous solution to the transient fixed source problem, the derivation of the solution method is focused on finding the particular solution efficiently. To avoid complicated particular solutions, the source distribution is approximated by quadratic polynomials and the transient source is constructed such that the error due to the quadratic approximation is minimized, In addition, this paper presents a new two-node solution scheme that is derived by imposing the constraint of current continuity at the interface corner points. The method is verified through a series of application to the NEACRP PWR rod ejection benchmark problems. 6 refs., 2 figs., 1 tab. (Author)

  2. Methods for estimating uncertainty in factor analytic solutions

    Directory of Open Access Journals (Sweden)

    P. Paatero

    2013-08-01

    Full Text Available EPA PMF version 5.0 and the underlying multilinear engine executable ME-2 contain three methods for estimating uncertainty in factor analytic models: classical bootstrap (BS, displacement of factor elements (DISP, and bootstrap enhanced by displacement of factor elements (BS-DISP. The goal of these methods is to capture the uncertainty of PMF analyses due to random errors and rotational ambiguity. It is shown that the three methods complement each other: depending on characteristics of the data set, one method may provide better results than the other two. Results are presented using synthetic data sets, including interpretation of diagnostics, and recommendations are given for parameters to report when documenting uncertainty estimates from EPA PMF or ME-2 applications.

  3. Study of plasmonic slot waveguides with a nonlinear metamaterial core: semi-analytical and numerical methods

    CERN Document Server

    Elsawy, Mahmoud M R

    2016-01-01

    Two distinct models are developed to investigate the transverse magnetic stationary solutions propagating in one-dimensional anisotropic nonlinear plasmonic structures made from a nonlinear metamaterial core of Kerr-type embedded between two semi-infinite metal claddings. The first model is semi-analytical, in which we assumed that the anisotropic nonlinearity depends only on the transverse component of the electric field and that the nonlinear refractive index modification is small compared to the linear one. This method allows us to derive analytically the field profiles and the nonlinear dispersion relations in terms of the Jacobi elliptical functions. The second model is fully numerical, it is based on the finite-element method in which all the components of the electric field are considered in the Kerr-type nonlinearity with no presumptions on the nonlinear refractive index change. Our finite-element based model is valid beyond weak nonlinearity regime and generalize the well-known single-component fixed...

  4. Stiffness matrix formulation for double row angular contact ball bearings: Analytical development and validation

    Science.gov (United States)

    Gunduz, Aydin; Singh, Rajendra

    2013-10-01

    Though double row angular contact ball bearings are widely used in industrial, automotive, and aircraft applications, the scientific literature on double row bearings is sparse. It is also shown that the stiffness matrices of two single row bearings may not be simply superposed to obtain the stiffness matrix of a double row bearing. To overcome the deficiency in the literature, a new, comprehensive, analytical approach is proposed based on the Hertzian theory for back-to-back, face-to-face, and tandem arrangements. The elements of the five-dimensional stiffness matrix for double row angular contact ball bearings are computed given either the mean bearing displacement or the mean load vector. The diagonal elements of the proposed stiffness matrix are verified with a commercial code for all arrangements under three loading scenarios. Some changes in stiffness coefficients are investigated by varying critical kinematic and geometric parameters to provide more insight. Finally, the calculated natural frequencies of a shaft-bearing experiment are successfully compared with measurements, thus validating the proposed stiffness formulation. For double row angular contact ball bearings, the moment stiffness and cross-coupling stiffness terms are significant, and the contact angle changes under loads. The proposed formulation is also valid for paired (duplex) bearings which behave as an integrated double row unit when the surrounding structural elements are sufficiently rigid.

  5. Analytical Validation of a Portable Mass Spectrometer Featuring Interchangeable, Ambient Ionization Sources for High Throughput Forensic Evidence Screening

    Science.gov (United States)

    Lawton, Zachary E.; Traub, Angelica; Fatigante, William L.; Mancias, Jose; O'Leary, Adam E.; Hall, Seth E.; Wieland, Jamie R.; Oberacher, Herbert; Gizzi, Michael C.; Mulligan, Christopher C.

    2016-12-01

    Forensic evidentiary backlogs are indicative of the growing need for cost-effective, high-throughput instrumental methods. One such emerging technology that shows high promise in meeting this demand while also allowing on-site forensic investigation is portable mass spectrometric (MS) instrumentation, particularly that which enables the coupling to ambient ionization techniques. While the benefits of rapid, on-site screening of contraband can be anticipated, the inherent legal implications of field-collected data necessitates that the analytical performance of technology employed be commensurate with accepted techniques. To this end, comprehensive analytical validation studies are required before broad incorporation by forensic practitioners can be considered, and are the focus of this work. Pertinent performance characteristics such as throughput, selectivity, accuracy/precision, method robustness, and ruggedness have been investigated. Reliability in the form of false positive/negative response rates is also assessed, examining the effect of variables such as user training and experience level. To provide flexibility toward broad chemical evidence analysis, a suite of rapidly-interchangeable ion sources has been developed and characterized through the analysis of common illicit chemicals and emerging threats like substituted phenethylamines.

  6. Random Qualitative Validation: A Mixed-Methods Approach to Survey Validation

    Science.gov (United States)

    Van Duzer, Eric

    2012-01-01

    The purpose of this paper is to introduce the process and value of Random Qualitative Validation (RQV) in the development and interpretation of survey data. RQV is a method of gathering clarifying qualitative data that improves the validity of the quantitative analysis. This paper is concerned with validity in relation to the participants'…

  7. Implementation of the Maximum Entropy Method for Analytic Continuation

    CERN Document Server

    Levy, Ryan; Gull, Emanuel

    2016-01-01

    We present $\\texttt{Maxent}$, a tool for performing analytic continuation of spectral functions using the maximum entropy method. The code operates on discrete imaginary axis datasets (values with uncertainties) and transforms this input to the real axis. The code works for imaginary time and Matsubara frequency data and implements the 'Legendre' representation of finite temperature Green's functions. It implements a variety of kernels, default models, and grids for continuing bosonic, fermionic, anomalous, and other data. Our implementation is licensed under GPLv2 and extensively documented. This paper shows the use of the programs in detail.

  8. Higher geometry an introduction to advanced methods in analytic geometry

    CERN Document Server

    Woods, Frederick S

    2005-01-01

    For students of mathematics with a sound background in analytic geometry and some knowledge of determinants, this volume has long been among the best available expositions of advanced work on projective and algebraic geometry. Developed from Professor Woods' lectures at the Massachusetts Institute of Technology, it bridges the gap between intermediate studies in the field and highly specialized works.With exceptional thoroughness, it presents the most important general concepts and methods of advanced algebraic geometry (as distinguished from differential geometry). It offers a thorough study

  9. Method of Analytic Evolution of Flat Distribution Amplitudes in QCD

    CERN Document Server

    Tandogan, Asli

    2011-01-01

    A new analytical method of performing ERBL evolution is described. The main goal is to develop an approach that works for distribution amplitudes that do not vanish at the end points, for which the standard method of expansion in Gegenbauer polynomials is inefficient. Two cases of the initial DA are considered: a purely flat DA, given by the same constant for all x, and an antisymmetric DA given by opposite constants for x 1/2. For a purely flat DA, the evolution is governed by an overall (x (1-x))^t dependence on the evolution parameter t times a factor that was calculated as an expansion in t. For an antisymmetric flat DA, an extra overall factor |1-2x|^{2t} appears due to a jump at x=1/2. A good convergence was observed in the t < 1/2 region. For larger t, one can use the standard method of the Gegenbauer expansion.

  10. The evolution of analytical chemistry methods in foodomics.

    Science.gov (United States)

    Gallo, Monica; Ferranti, Pasquale

    2016-01-08

    The methodologies of food analysis have greatly evolved over the past 100 years, from basic assays based on solution chemistry to those relying on the modern instrumental platforms. Today, the development and optimization of integrated analytical approaches based on different techniques to study at molecular level the chemical composition of a food may allow to define a 'food fingerprint', valuable to assess nutritional value, safety and quality, authenticity and security of foods. This comprehensive strategy, defined foodomics, includes emerging work areas such as food chemistry, phytochemistry, advanced analytical techniques, biosensors and bioinformatics. Integrated approaches can help to elucidate some critical issues in food analysis, but also to face the new challenges of a globalized world: security, sustainability and food productions in response to environmental world-wide changes. They include the development of powerful analytical methods to ensure the origin and quality of food, as well as the discovery of biomarkers to identify potential food safety problems. In the area of nutrition, the future challenge is to identify, through specific biomarkers, individual peculiarities that allow early diagnosis and then a personalized prognosis and diet for patients with food-related disorders. Far from the aim of an exhaustive review of the abundant literature dedicated to the applications of omic sciences in food analysis, we will explore how classical approaches, such as those used in chemistry and biochemistry, have evolved to intersect with the new omics technologies to produce a progress in our understanding of the complexity of foods. Perhaps most importantly, a key objective of the review will be to explore the development of simple and robust methods for a fully applied use of omics data in food science.

  11. Using analytic network process for evaluating mobile text entry methods.

    Science.gov (United States)

    Ocampo, Lanndon A; Seva, Rosemary R

    2016-01-01

    This paper highlights a preference evaluation methodology for text entry methods in a touch keyboard smartphone using analytic network process (ANP). Evaluation of text entry methods in literature mainly considers speed and accuracy. This study presents an alternative means for selecting text entry method that considers user preference. A case study was carried out with a group of experts who were asked to develop a selection decision model of five text entry methods. The decision problem is flexible enough to reflect interdependencies of decision elements that are necessary in describing real-life conditions. Results showed that QWERTY method is more preferred than other text entry methods while arrangement of keys is the most preferred criterion in characterizing a sound method. Sensitivity analysis using simulation of normally distributed random numbers under fairly large perturbation reported the foregoing results reliable enough to reflect robust judgment. The main contribution of this paper is the introduction of a multi-criteria decision approach in the preference evaluation of text entry methods.

  12. Validating and Determining the Weight of Items Used for Evaluating Clinical Governance Implementation Based on Analytic Hierarchy Process Model

    Directory of Open Access Journals (Sweden)

    Elaheh Hooshmand

    2015-10-01

    Full Text Available Background The purpose of implementing a system such as Clinical Governance (CG is to integrate, establish and globalize distinct policies in order to improve quality through increasing professional knowledge and the accountability of healthcare professional toward providing clinical excellence. Since CG is related to change, and change requires money and time, CG implementation has to be focused on priority areas that are in more dire need of change. The purpose of the present study was to validate and determine the significance of items used for evaluating CG implementation. Methods The present study was descriptive-quantitative in method and design. Items used for evaluating CG implementation were first validated by the Delphi method and then compared with one another and ranked based on the Analytical Hierarchy Process (AHP model. Results The items that were validated for evaluating CG implementation in Iran include performance evaluation, training and development, personnel motivation, clinical audit, clinical effectiveness, risk management, resource allocation, policies and strategies, external audit, information system management, research and development, CG structure, implementation prerequisites, the management of patients’ non-medical needs, complaints and patients’ participation in the treatment process. The most important items based on their degree of significance were training and development, performance evaluation, and risk management. The least important items included the management of patients’ non-medical needs, patients’ participation in the treatment process and research and development. Conclusion The fundamental requirements of CG implementation included having an effective policy at national level, avoiding perfectionism, using the expertise and potentials of the entire country and the coordination of this model with other models of quality improvement such as accreditation and patient safety.

  13. The Value of Qualitative Methods in Social Validity Research

    Science.gov (United States)

    Leko, Melinda M.

    2014-01-01

    One quality indicator of intervention research is the extent to which the intervention has a high degree of social validity, or practicality. In this study, I drew on Wolf's framework for social validity and used qualitative methods to ascertain five middle schoolteachers' perceptions of the social validity of System 44®--a phonics-based reading…

  14. Method validation for chemical composition determination by electron microprobe with wavelength dispersive spectrometer

    Science.gov (United States)

    Herrera-Basurto, R.; Mercader-Trejo, F.; Muñoz-Madrigal, N.; Juárez-García, J. M.; Rodriguez-López, A.; Manzano-Ramírez, A.

    2016-07-01

    The main goal of method validation is to demonstrate that the method is suitable for its intended purpose. One of the advantages of analytical method validation is translated into a level of confidence about the measurement results reported to satisfy a specific objective. Elemental composition determination by wavelength dispersive spectrometer (WDS) microanalysis has been used over extremely wide areas, mainly in the field of materials science, impurity determinations in geological, biological and food samples. However, little information is reported about the validation of the applied methods. Herein, results of the in-house method validation for elemental composition determination by WDS are shown. SRM 482, a binary alloy Cu-Au of different compositions, was used during the validation protocol following the recommendations for method validation proposed by Eurachem. This paper can be taken as a reference for the evaluation of the validation parameters more frequently requested to get the accreditation under the requirements of the ISO/IEC 17025 standard: selectivity, limit of detection, linear interval, sensitivity, precision, trueness and uncertainty. A model for uncertainty estimation was proposed including systematic and random errors. In addition, parameters evaluated during the validation process were also considered as part of the uncertainty model.

  15. Migração de β-caprolactama de embalagens contendo poliamida 6 para simulante ácido acético 3% e validação do método analítico β-Caprolactam migration from polyamide 6 packaging into 3% acetic acid food simulant and validation of the analytical method

    Directory of Open Access Journals (Sweden)

    Juliana Silva Félix

    2007-08-01

    Full Text Available Este trabalho teve como objetivo desenvolver e validar método analítico para determinar ε-caprolactama no simulante de alimentos solução de ácido acético 3% e estudar sua migração de embalagens contendo poliamida 6 para o simulante em contato. Foi empregada a cromatografia gasosa usando ε-caprolactama como padrão analítico e 2-azociclononanona como padrão interno. A linearidade esteve entre 1,60 e 640,00 µg de ε-caprolactama.mL-1 de simulante, com coeficiente de correlação 0,9999. Os limites de detecção e de quantificação do método foram 0,24 e 1,60 ng, respectivamente. A precisão do método revelou valores de coeficiente de variação menores que 4,3% e a avaliação da exatidão mostrou recuperação de 100 a 106%. O método demonstrou ser eficaz para quantificar ε-caprolactama no simulante, apresentando ampla linearidade, boa precisão e exatidão. No ensaio de migração, embalagens contendo poliamida 6 foram colocadas em tubos de vidro com 10 mL do simulante, que foram hermeticamente fechados e acondicionados a 40 ± 1 °C durante 10 dias. O ensaio de migração foi realizado por imersão total. A quantidade de ε-caprolactama migrada variou de 7,8 a 10,5 e de 6,9 a 7,6 mg.kg-1 de simulante para as embalagens destinadas aos produtos cárneos e queijos, respectivamente. Todas as embalagens atenderam às exigências da Legislação Brasileira para migração de ε-caprolactama.The aim of this work was to develop and validate an analytical method to determine ε-caprolactam in 3% acetic acid solution and to study its migration from polyamide 6 into food simulant. Gas chromatography was used with ε-caprolactam as an analytical standard and 2-azacyclononanone as an internal standard. The linearity was obtained by the concentration range of 1.60 to 640.00 µg.mL-1, with a correlation coefficient of 0.9999. Detection and quantification limits of the method were 0.24 ng and 1.60 ng, respectively. Relative standard

  16. The use of graphic-analytical method in investment design

    Directory of Open Access Journals (Sweden)

    Musatova Tatiana

    2016-04-01

    Full Text Available We investigate the possibility of using the network planning method for the goals and objectives of the investment project. The author suggests a network model of implementing the investment project related to the manufacture of aluminum structures. Insufficient study of adaptation of methodological issues of organization of technological processes to the investment project of socio-economic activities has led to the relevance and identified the purpose of the present study. The presented network model allows project participants to optimize the time and costs of various types of project resources. It includes the calculation of the parameters of the network schedule and the actual model of interrelated events and activities. Scientific and practical significance of the results of research is related to the possibility of practical application of graphic-analytical method for the preparation of technical and economic documentation for the investment project.

  17. Analytic continuation average spectrum method for transport in quantum liquids

    Energy Technology Data Exchange (ETDEWEB)

    Kletenik-Edelman, Orly [School of Chemistry, Sackler Faculty of Exact Sciences, Tel Aviv University, Tel Aviv 69978 (Israel); Rabani, Eran, E-mail: rabani@tau.ac.il [School of Chemistry, Sackler Faculty of Exact Sciences, Tel Aviv University, Tel Aviv 69978 (Israel); Reichman, David R. [Department of Chemistry, Columbia University, 3000 Broadway, New York, NY 10027 (United States)

    2010-05-12

    Recently, we have applied the analytic continuation averaged spectrum method (ASM) to calculate collective density fluctuations in quantum liquid . Unlike the maximum entropy (MaxEnt) method, the ASM approach is capable of revealing resolved modes in the dynamic structure factor in agreement with experiments. In this work we further develop the ASM to study single-particle dynamics in quantum liquids with dynamical susceptibilities that are characterized by a smooth spectrum. Surprisingly, we find that for the power spectrum of the velocity autocorrelation function there are pronounced differences in comparison with the MaxEnt approach, even for this simple case of smooth unimodal dynamic response. We show that for liquid para-hydrogen the ASM is closer to the centroid molecular dynamics (CMD) result while for normal liquid helium it agrees better with the quantum mode coupling theory (QMCT) and with the MaxEnt approach.

  18. Introduction to Analytical Methods for Internal Combustion Engine Cam Mechanisms

    CERN Document Server

    Williams, J J

    2013-01-01

    Modern design methods of Automotive Cam Design require the computation of a range of parameters. This book provides a logical sequence of steps for the derivation of the relevant equations from first principles, for the more widely used cam mechanisms. Although originally derived for use in high performance engines, this work is equally applicable to the design of mass produced automotive and other internal combustion engines.   Introduction to Analytical Methods for Internal Combustion Engine Cam Mechanisms provides the equations necessary for the design of cam lift curves with an associated smooth acceleration curve. The equations are derived for the kinematics and kinetics of all the mechanisms considered, together with those for cam curvature and oil entrainment velocity. This permits the cam shape, all loads, and contact stresses to be evaluated, and the relevant tribology to be assessed. The effects of asymmetry on the manufacture of cams for finger follower and offset translating curved followers is ...

  19. VALIDATED SPECTROPHOTMETRIC METHOD FOR THE DETERMINATION OF SALBUTAMOL SULPHATE IN BULK AND PHARMACEUTICAL DOSAGE FORMS

    Directory of Open Access Journals (Sweden)

    Eswarudu.M.M

    2012-04-01

    Full Text Available A new, simple, accurate and sensitive spectrophotometric method has been developed for the estimation of Salbutamol sulphate in bulk and in pharmaceutical formulations. Salbutamol sulphate shows ʎ max at 292 nm. The drug follows the beer’s lambert’s law in the concentration range of 20-100µ ml. the method was validated by following the analytical performance parameters as suggested by the international conference on harmonization which included accuracy, precision, linearity. All validation parameters were with in the acceptable range. The developed method was successfully applied to estimate the amount of Salbutamol sulphate in bulk and pharmaceutical dosage forms.

  20. GenoSets: visual analytic methods for comparative genomics.

    Directory of Open Access Journals (Sweden)

    Aurora A Cain

    Full Text Available Many important questions in biology are, fundamentally, comparative, and this extends to our analysis of a growing number of sequenced genomes. Existing genomic analysis tools are often organized around literal views of genomes as linear strings. Even when information is highly condensed, these views grow cumbersome as larger numbers of genomes are added. Data aggregation and summarization methods from the field of visual analytics can provide abstracted comparative views, suitable for sifting large multi-genome datasets to identify critical similarities and differences. We introduce a software system for visual analysis of comparative genomics data. The system automates the process of data integration, and provides the analysis platform to identify and explore features of interest within these large datasets. GenoSets borrows techniques from business intelligence and visual analytics to provide a rich interface of interactive visualizations supported by a multi-dimensional data warehouse. In GenoSets, visual analytic approaches are used to enable querying based on orthology, functional assignment, and taxonomic or user-defined groupings of genomes. GenoSets links this information together with coordinated, interactive visualizations for both detailed and high-level categorical analysis of summarized data. GenoSets has been designed to simplify the exploration of multiple genome datasets and to facilitate reasoning about genomic comparisons. Case examples are included showing the use of this system in the analysis of 12 Brucella genomes. GenoSets software and the case study dataset are freely available at http://genosets.uncc.edu. We demonstrate that the integration of genomic data using a coordinated multiple view approach can simplify the exploration of large comparative genomic data sets, and facilitate reasoning about comparisons and features of interest.

  1. An analytic method to compute star cluster luminosity statistics

    Science.gov (United States)

    da Silva, Robert L.; Krumholz, Mark R.; Fumagalli, Michele; Fall, S. Michael

    2014-03-01

    The luminosity distribution of the brightest star clusters in a population of galaxies encodes critical pieces of information about how clusters form, evolve and disperse, and whether and how these processes depend on the large-scale galactic environment. However, extracting constraints on models from these data is challenging, in part because comparisons between theory and observation have traditionally required computationally intensive Monte Carlo methods to generate mock data that can be compared to observations. We introduce a new method that circumvents this limitation by allowing analytic computation of cluster order statistics, i.e. the luminosity distribution of the Nth most luminous cluster in a population. Our method is flexible and requires few assumptions, allowing for parametrized variations in the initial cluster mass function and its upper and lower cutoffs, variations in the cluster age distribution, stellar evolution and dust extinction, as well as observational uncertainties in both the properties of star clusters and their underlying host galaxies. The method is fast enough to make it feasible for the first time to use Markov chain Monte Carlo methods to search parameter space to find best-fitting values for the parameters describing cluster formation and disruption, and to obtain rigorous confidence intervals on the inferred values. We implement our method in a software package called the Cluster Luminosity Order-Statistic Code, which we have made publicly available.

  2. Desenvolvimento e validação de método analítico para nistatina creme vaginal por cromatografia líquida de alta eficiência Development and validation of an analytical method for Nystatin vaginal cream by high performance liquid chromatography

    Directory of Open Access Journals (Sweden)

    Zênia Maria Maciel Lavra

    2008-12-01

    1.0 mL/minute and wavelength of 305 nm. The validated method showed to be accurate, precise, robust, linear and specific, in addition to being fast and practical, able to be used for analytic dosing of nystatin vaginal cream.

  3. Assessing Partnership Alternatives in an IT Network Employing Analytical Methods

    Directory of Open Access Journals (Sweden)

    Vahid Reza Salamat

    2016-01-01

    Full Text Available One of the main critical success factors for the companies is their ability to build and maintain an effective collaborative network. This is more critical in the IT industry where the development of sustainable competitive advantage requires an integration of various resources, platforms, and capabilities provided by various actors. Employing such a collaborative network will dramatically change the operations management and promote flexibility and agility. Despite its importance, there is a lack of an analytical tool on collaborative network building process. In this paper, we propose an optimization model employing AHP and multiobjective programming for collaborative network building process based on two interorganizational relationships’ theories, namely, (i transaction cost theory and (ii resource-based view, which are representative of short-term and long-term considerations. The five different methods were employed to solve the formulation and their performances were compared. The model is implemented in an IT company who was in process of developing a large-scale enterprise resource planning (ERP system. The results show that the collaborative network formed through this selection process was more efficient in terms of cost, time, and development speed. The framework offers novel theoretical underpinning and analytical solutions and can be used as an effective tool in selecting network alternatives.

  4. An analytically based numerical method for computing view factors in real urban environments

    Science.gov (United States)

    Lee, Doo-Il; Woo, Ju-Wan; Lee, Sang-Hyun

    2016-11-01

    A view factor is an important morphological parameter used in parameterizing in-canyon radiative energy exchange process as well as in characterizing local climate over urban environments. For realistic representation of the in-canyon radiative processes, a complete set of view factors at the horizontal and vertical surfaces of urban facets is required. Various analytical and numerical methods have been suggested to determine the view factors for urban environments, but most of the methods provide only sky-view factor at the ground level of a specific location or assume simplified morphology of complex urban environments. In this study, a numerical method that can determine the sky-view factors (ψ ga and ψ wa ) and wall-view factors (ψ gw and ψ ww ) at the horizontal and vertical surfaces is presented for application to real urban morphology, which are derived from an analytical formulation of the view factor between two blackbody surfaces of arbitrary geometry. The established numerical method is validated against the analytical sky-view factor estimation for ideal street canyon geometries, showing a consolidate confidence in accuracy with errors of less than 0.2 %. Using a three-dimensional building database, the numerical method is also demonstrated to be applicable in determining the sky-view factors at the horizontal (roofs and roads) and vertical (walls) surfaces in real urban environments. The results suggest that the analytically based numerical method can be used for the radiative process parameterization of urban numerical models as well as for the characterization of local urban climate.

  5. USING ANALYTIC HIERARCHY PROCESS (AHP METHOD IN RURAL DEVELOPMENT

    Directory of Open Access Journals (Sweden)

    Tülay Cengiz

    2003-04-01

    Full Text Available Rural development is a body of economical and social policies towards improving living conditions in rural areas through enabling rural population to utilize economical, social, cultural and technological blessing of city life in place, without migrating. As it is understood from this description, rural development is a very broad concept. Therefore, in development efforts problem should be stated clearly, analyzed and many criterias should be evaluated by experts. Analytic Hierarchy Process (AHP method can be utilized at there stages of development efforts. AHP methods is one of multi-criteria decision method. After degrading a problem in smaller pieces, relative importance and level of importance of two compared elements are determined. It allows evaluation of quality and quantity factors. At the same time, it permits utilization of ideas of many experts and use them in decision process. Because mentioned features of AHP method, it could be used in rural development works. In this article, cultural factors, one of the important components of rural development is often ignored in many studies, were evaluated as an example. As a result of these applications and evaluations, it is concluded that AHP method could be helpful in rural development efforts.

  6. THERE IS NO MATHEMATICAL VALIDITY FOR USING FUZZY NUMBER CRUNCHING IN THE ANALYTIC HIERARCHY PROCESS

    Institute of Scientific and Technical Information of China (English)

    Thomas L. SAATY

    2006-01-01

    Fuzzy logic has difficulty producing valid answers in decision-making. Absent are theorems to prove that it works to produce results already known that are being estimated with judgments by transforming such judgments numerically. The numerical representation of judgments in the AHP is already fuzzy. Making fuzzy judgments more fuzzy does not lead to a better more valid outcome and it often leads to a worse one. The compatibility index of the AHP is used to illustrate how the answers obtained by fuzzifying AHP judgments do not produce better results than direct derivation of the principal eigenvector. Other authors who did experiments with given data in decision making quoted in the conclusions section of the paper, have observed that fuzzy sets gives the poorest answers among all methods used to derive best decisions.

  7. Validation of an analytical compressed elastic tube model for acoustic wave propagation

    Science.gov (United States)

    Van Hirtum, A.; Blandin, R.; Pelorson, X.

    2015-12-01

    Acoustic wave propagation through a compressed elastic tube is a recurrent problem in engineering. Compression of the tube is achieved by pinching it between two parallel bars so that the pinching effort as well as the longitudinal position of pinching can be controlled. A stadium-based geometrical tube model is combined with a plane wave acoustic model in order to estimate acoustic wave propagation through the elastic tube as a function of pinching effort, pinching position, and outlet termination (flanged or unflanged). The model outcome is validated against experimental data obtained in a frequency range from 3.5 kHz up to 10 kHz by displacing an acoustic probe along the tube's centerline. Due to plane wave model assumptions and the decrease of the lowest higher order mode cut-on frequency with increasing pinching effort, the difference between modeled and measured data is analysed in three frequency bands, up to 5 kHz, 8 kHz, and 9.5 kHz, respectively. It is seen that the mean and standard error within each frequency band do not significantly vary with pinching effort, pinching position, or outlet termination. Therefore, it is concluded that the analytical tube model is suitable to approximate the elastic tube geometry when modeling acoustic wave propagation through the pinched elastic tube with either flanged or unflanged termination.

  8. Development and validation of a path analytic model of students' performance in chemistry

    Science.gov (United States)

    Anamuah-Mensah, Jophus; Erickson, Gaalen; Gaskell, Jim

    This article reports the development and validation of an integrated model of performance on a chemical concept - volumetric analysis. From the chemical literature a path-analytic model of performance on volumetric analysis calculation was postulated based on studies utilizing the proportional reasoning schema of Piaget and the Cumulative learning theory of Gagne. This integrated model hypothesized some relationships among the variables: direct proportional reasoning, inverse proportional reasoning, prerequisite concepts (content) and performance on volumetric analysis calculations. This model was postulated for the two groups of students involved in the study - that is those who use algorithms with understanding and those who use algorithms without understanding. Two hundred and sixty-five grade twelve chemistry students in eight schools (14 classes) in the lower mainland of British Columbia, Canada participated fully in the study. With the exception of the test on volumetric analysis calculations all the other tests were administered prior to the teaching of the unit on volumetric analysis. The results of the study indicate that for subjects using algorithms without understanding, their performance on VA problems is not influenced by proportional reasoning strategies while for those who use algorithms with understanding, their performance is influenced by proportional reasoning strategies.

  9. Analytical methods for residual solvents determination in pharmaceutical products.

    Science.gov (United States)

    Grodowska, Katarzyna; Parczewski, Andrzej

    2010-01-01

    Residual solvents (RS) are not desirable substances in the final pharmaceutical product and their acceptable limits have been published in pharmacopoeias and ICH guidelines. The intension of this paper was to review and discuss some of the current analytical procedures including gas chromatographic (GC) and other alternative techniques which are used for residual solvents determination. GC methods have been developed to monitor this kind of impurities routinely. The most popular techniques of sample introduction into the gas chromatograph include direct injection, static or dynamic headspace, solid-phase microextraction and single drop microextraction. Different separation techniques like two dimensional chromatography or multicapillary chromatography were compared with classical separation mode with use of single capillary column. Also alternative methodologies for residual solvents testing were discussed in this review. In conclusions, gas chromatography-based procedures were described as the most appropriate because of the lowest detection limits, ease of sample preparation and specificity.

  10. Analytical methods for volatile compounds in wheat bread.

    Science.gov (United States)

    Pico, Joana; Gómez, Manuel; Bernal, José; Bernal, José Luis

    2016-01-08

    Bread aroma is one of the main requirements for its acceptance by consumers, since it is one of the first attributes perceived. Sensory analysis, crucial to be correlated with human perception, presents limitations and needs to be complemented with instrumental analysis. Gas chromatography coupled to mass spectrometry is usually selected as the technique to determine bread volatile compounds, although proton-transfer reaction mass spectrometry begins also to be used to monitor aroma processes. Solvent extraction, supercritical fluid extraction and headspace analysis are the main options for the sample treatment. The present review focuses on the different sample treatments and instrumental alternatives reported in the literature to analyse volatile compounds in wheat bread, providing advantages and limitations. Usual parameters employed in these analytical methods are also described.

  11. Polymeric vehicles for topical delivery and related analytical methods.

    Science.gov (United States)

    Cho, Heui Kyoung; Cho, Jin Hun; Jeong, Seong Hoon; Cho, Dong Chul; Yeum, Jeong Hyun; Cheong, In Woo

    2014-04-01

    Recently a variety of polymeric vehicles, such as micelles, nanoparticles, and polymersomes, have been explored and some of them are clinically used to deliver therapeutic drugs through skin. In topical delivery, the polymeric vehicles as drug carrier should guarantee non-toxicity, long-term stability, and permeation efficacy for drugs, etc. For the development of the successful topical delivery system, it is of importance to develop the polymeric vehicles of well-defined intrinsic properties, such as molecular weights, HLB, chemical composition, topology, specific ligand conjugation and to investigate the effects of the properties on drug permeation behavior. In addition, the role of polymeric vehicles must be elucidated in in vitro and in vivo analyses. This article describes some important features of polymeric vehicles and corresponding analytical methods in topical delivery even though the application span of polymers has been truly broad in the pharmaceutical fields.

  12. Application of analytical methods in authentication and adulteration of honey.

    Science.gov (United States)

    Siddiqui, Amna Jabbar; Musharraf, Syed Ghulam; Choudhary, M Iqbal; Rahman, Atta-Ur-

    2017-02-15

    Honey is synthesized from flower nectar and it is famous for its tremendous therapeutic potential since ancient times. Many factors influence the basic properties of honey including the nectar-providing plant species, bee species, geographic area, and harvesting conditions. Quality and composition of honey is also affected by many other factors, such as overfeeding of bees with sucrose, harvesting prior to maturity, and adulteration with sugar syrups. Due to the complex nature of honey, it is often challenging to authenticate the purity and quality by using common methods such as physicochemical parameters and more specialized procedures need to be developed. This article reviews the literature (between 2000 and 2016) on the use of analytical techniques, mainly NMR spectroscopy, for authentication of honey, its botanical and geographical origin, and adulteration by sugar syrups. NMR is a powerful technique and can be used as a fingerprinting technique to compare various samples.

  13. Analytical validation for the HRMS detection of organochlorines in living marine mammals from biopsy microsamples

    Energy Technology Data Exchange (ETDEWEB)

    Ikonomou, M.G.; Crewe, N.F.; Fischer, M.; Smith, T.G. [Dept. of Fisheries and Oceans, Sidney, British Columbia (Canada)

    1995-12-31

    It has been demonstrated that marine mammals accumulate high concentrations of lipophilic organochlorine contaminants in blubber. As predators of the high trophic level they have also been used to evaluate contamination in the marine environment. Sampling of living marine mammals using a microsample (100 to 200 mg) biopsy dart technique offers a potentially invaluable chronicle in assessing levels and types of persistent environmental pollutants from a sample in which age, sex and other genetic information can additionally be ascertained. The authors have explored analytical methodology based on a high sensitivity detection system (HRGC/HRMS) which provides multi-residue determinations from biopsy dart microsamples. Lipid content and the concentrations of PCDDs, PCDFs and non-ortho and mono-ortho substituted PCBs were measured in 100 mg biopsy dart replicates taken from a killer whale carcass and in three strata of the blubber of that carcass. Statistically acceptable results were obtained from the dart replicates which compared very well with those of the blubber strata. Analytical data from 100 mg extractions from an established in house blubber CRM also compared well against a series of 2.5 g extractions of that CRM. The extraction and cleanup procedures used also allow for the determination of other organohalogen contaminants such as DDT and other pesticides, all the remaining PCBs, polychlorinated diphenylethers and brominated residues. The strengths and limitations of the analytical methodology and the biopsy dart as a sampling tool and pollution predicator will be illustrated in terms of method accuracy and precision, glassware and procedural blanks associated with each extraction batch, and the incorporation of an in house micro reference standard.

  14. Comparison of the Helicobacter Pylori Diagnosis Methods with Analytic Network Process

    Directory of Open Access Journals (Sweden)

    Hacer KONAKLI

    2015-11-01

    Full Text Available Helicobacter pylori is infecting %70-80 of the world’s population and is assumed to cause gastric diseases. Diagnosis of the bacteria is crucial for the treatment of the bacteria related infections. Histology, culture, urea breath test, stool antigen test some of the diagnosis methods each having specific strength and weaknesses as sensitivity, specificity, cost, easiness, time, effectiveness in the treatment and laboratory requirements. In this study, three of the commonly used H. pylori diagnosis methods: histology, culture and urea breath test, are evaluated with Analytic network process (ANP and the rank of the criteria and alternatives are obtained. The evaluation of the methods and the rank of the diagnosis methods can reduce time, cost, and validity of the test results.

  15. 40 CFR 260.21 - Petitions for equivalent testing or analytical methods.

    Science.gov (United States)

    2010-07-01

    ... analytical methods. 260.21 Section 260.21 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY... Petitions for equivalent testing or analytical methods. (a) Any person seeking to add a testing or analytical method to part 261, 264, or 265 of this chapter may petition for a regulatory amendment under...

  16. 21 CFR 530.40 - Safe levels and availability of analytical methods.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 6 2010-04-01 2010-04-01 false Safe levels and availability of analytical methods... Safe levels and availability of analytical methods. (a) In accordance with § 530.22, the following safe... accordance with § 530.22, the following analytical methods have been accepted by FDA:...

  17. CT hepatic perfusion measurement: Comparison of three analytic methods

    Energy Technology Data Exchange (ETDEWEB)

    Kanda, Tomonori [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan); Yoshikawa, Takeshi, E-mail: yoshikawa0816@aol.com [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan); Ohno, Yoshiharu; Kanata, Naoki; Koyama, Hisanobu; Takenaka, Daisuke; Sugimura, Kazuro [Department of Radiology, Kobe University Graduate School of Medicine, 7-5-2 Kusunokicho, Chuoku, Kobe 650-0017 (Japan)

    2012-09-15

    Objectives: To compare the efficacy of three analytic methods, maximum slope (MS), dual-input single-compartment model (CM) and deconvolution (DC), for CT measurements of hepatic perfusion and assess the effects of extra-hepatic systemic factors. Materials and methods: Eighty-eight patients who were suspected of having metastatic liver tumors underwent hepatic CT perfusion. The scans were performed at the hepatic hilum 7–77 s after administration of contrast material. Hepatic arterial and portal perfusions (HAP and HPP, ml/min/100 ml) and arterial perfusion fraction (APF, %) were calculated with the three methods, followed by correlation assessment. Partial correlation analysis was used to assess the effects on hepatic perfusion values by various factors such as age, sex, risk of cardiovascular diseases, arrival time of contrast material at abdominal aorta, transit time from abdominal aorta to hepatic parenchyma, and liver dysfunction. Results: Mean HAP of MS was significantly higher than DC. HPP of CM was significantly higher than MS and CM, and HPP of MS was significantly higher than DC. There was no significant difference in APF. HAP and APF showed significant and moderate correlations among the methods. HPP showed significant and moderate correlations between CM and DC, and poor correlation between MS and CM or DC. All methods showed weak correlations between HAP or APF and age or sex. Finally, MS showed weak correlations between HAP or HPP and arrival time or cardiovascular risks. Conclusions: Hepatic perfusion values arrived at with the three methods are not interchangeable. CM and DC are less susceptible to extra-hepatic systemic factors.

  18. Graph-Analytical Method of Determining Impedance in Electrical Transformers

    Directory of Open Access Journals (Sweden)

    Zorica Bogicevic

    2015-01-01

    Full Text Available This paper presents a graph-analytical method for determining the electrical impedance of alternate energy sources, especially small power transformers and current transformers in electric networks. Unlike conventional short-circuit and idle tests, according to proposed method, in this paper, transformer parameters are determined in a new way, which is based on measurement of voltages and currents on the active and reactive load (inductive or capacitive. The effectiveness of the proposed model was verified using an adapted simulation in the software package MATLAB Simulink. The simulation was performed for three types of ABB transformers with a 100% load. Simulation results were obtained for power transformers: Sn1=1 [MVA], Sn2=2 [MVA], Sn3=3.15 [MVA]. If we compare measurement result values of RT, XT, which are contained in a brochure for ABB transformers and those obtained through simulation, different tolerances are obtained. For reactance results, deviations are up to 20% for all three tested transformers. For results of active resistance tolerances are up to 5% for all three tested transformers. This method can be used not only to determine the active and inductive AC power source parameters but also to determine and analyze the impendence of electrical sources with high frequencies.

  19. Development and Validation of a UV - Spectrophotometric Method for Quantification of Atorvastatin in Tablets

    Directory of Open Access Journals (Sweden)

    Mondal A

    2012-01-01

    Full Text Available A UV-spectrophotometric method has been developed for the quantitativeestimation of atorvastatin in tablet. The present study describes development and validation of UV-spectroscopic method for estimationof atorvastatin in tablet dosage form and validation of newlydeveloped method. During development of analytical method methanol:phosphate buffer (20:80,methanol:water(20:80,methanol:water (50:50,acetonitrile:water (10:90were tried but drug was found to be solublein methanol:water (50:50. Standard stock solution was prepared in methanol: water (50:50. The detection wave length (λmax was found tobe 248nm.Calibration curves were prepared.The proposed method obeysBeer's law in the range of 5-15μg/ml. Absorption maxima was determinedwith 10 μg/ml by scanning in the range of 200-400nm.Percent recoverystudies are in the range of 98.78%-100.36%. The method was validated in terms specificity,linearity,accuracy,range,precision,repeatability,robustness,system suitability,stability of analytical solution.Results of analysis were validated statistically and by specificity studies.From that it was observed that there is no interference of blank,excipients during the estimation of drug in formulation. This showsthe adaptability of the method for routine estimation of atorvastatinin tablet dosage form.

  20. On the construction of a new solvable model and validity of many-body approximation methods

    Science.gov (United States)

    Zettili, Nouredine; Villars, Felix M. H.

    1987-07-01

    This work deals both with the construction of a new analytically solvable model and with the quantitative test of the time-dependent Hartree-Fock (TDHF) method. First, we construct a new analytically solvable model, which serves as a testing ground for the various many-body approximation methods. The construction is based on two vector operators that are the generators of a Lie algebra. The model consists of a one-dimensional system of two distinguishable sets of fermions interacting via a schematic two-body force. The model has a simple analytic energy spectrum. Second, we use this model to test the validity of the TDHF approximation. Exact eigenvalues are compared with the corresponding solutions of the TDHF method. The TDHF approximation is shown to be reasonably accurate in the description of the system's eigenstates.

  1. On the construction of a new solvable model and validity of many-body approximation methods

    Energy Technology Data Exchange (ETDEWEB)

    Zettili, N.; Villars, F.M.H.

    1987-07-20

    This work deals both with the construction of a new analytically solvable model and with the quantitative test of the time-dependent Hartree-Fock (TDHF) method. First, we construct a new analytically solvable model, which serves as a testing ground for the various many-body approximation methods. The construction is based on two vector operators that are the generators of a Lie algebra. The model consists of a one-dimensional system of two distinguishable sets of fermions interacting via a schematic two-body force. The model has a simple analytic energy spectrum. Second, we use this model to test the validity of the TDHF approximation. Exact eigenvalues are compared with the corresponding solutions of the TDHF method. The TDHF approximation is shown to be reasonably accurate in the description of the system's eigenstates.

  2. Recent trends in analytical methods to determine new psychoactive substances in hair.

    Science.gov (United States)

    Kyriakou, Chrystalla; Pellegrini, Manuela; García-Algar, Oscar; Marinelli, Enrico; Zaami, Simona

    2016-11-11

    New Psychoactive Substances (NPS) belong to several chemical classes, including phenethylamines, piperazines, synthetic cathinones and synthetic cannabinoids. Development and validation of analytical methods for the determination of NPS both in traditional and alternative matrices is of crucial importance to study drug metabolism and to associate consumption to clinical outcomes and eventual intoxication symptoms. Among different biological matrices, hair is the one with the widest time window to investigate drug-related history and demonstrate past intake. The aim of this paper was to overview the trends of the rapidly evolving analytical methods for the determination of NPS in hair and the usefulness of these methods when applied to real cases. A number of rapid and sensitive methods for the determination of NPS in hair matrix has been recently published, most of them using liquid chromatography coupled to mass spectrometry. Hair digestion and subsequent solid phase extraction or liquid-liquid extraction were described as well as extraction in organic solvents. For most of the methods limits of quantification at picogram per milligram hair were obtained. The measured concentrations for most of the NPS in real samples were in the range of picograms of drug per milligram of hair. Interpretation of the results and lack of cut-off values for the discrimination between chronic consumption and occasional use or external contamination are still challenging. Methods for the determination of NPS in hair are continually emerging to include as many NPS as possible due to the great demand for their detection.

  3. Thrust measurement method verification and analytical studies on a liquid-fueled pulse detonation engine

    Institute of Scientific and Technical Information of China (English)

    Lu Jie; Zheng Longxi; Wang Zhiwu; Peng Changxin; Chen Xinggu

    2014-01-01

    In order to test the feasibility of a new thrust stand system based on impulse thrust mea-surement method, a liquid-fueled pulse detonation engine (PDE) is designed and built. Thrust per-formance of the engine is obtained by direct thrust measurement with a force transducer and indirect thrust measurement with an eddy current displacement sensor (ECDS). These two sets of thrust data are compared with each other to verify the accuracy of the thrust performance. Then thrust data measured by the new thrust stand system are compared with the verified thrust data to test its feasibility. The results indicate that thrust data from the force transducer and ECDS system are consistent with each other within the range of measurement error. Though the thrust data from the impulse thrust measurement system is a litter lower than that from the force transducer due to the axial momentum losses of the detonation jet, the impulse thrust measurement method is valid when applied to measure the averaged thrust of PDE. Analytical models of PDE are also discussed in this paper. The analytical thrust performance is higher than the experimental data due to ignor-ing the losses during the deflagration to detonation transition process. Effect of equivalence ratio on the engine thrust performance is investigated by utilizing the modified analytical model. Thrust reaches maximum at the equivalence ratio of about 1.1.

  4. Thrust measurement method verification and analytical studies on a liquid-fueled pulse detonation engine

    Directory of Open Access Journals (Sweden)

    Lu Jie

    2014-06-01

    Full Text Available In order to test the feasibility of a new thrust stand system based on impulse thrust measurement method, a liquid-fueled pulse detonation engine (PDE is designed and built. Thrust performance of the engine is obtained by direct thrust measurement with a force transducer and indirect thrust measurement with an eddy current displacement sensor (ECDS. These two sets of thrust data are compared with each other to verify the accuracy of the thrust performance. Then thrust data measured by the new thrust stand system are compared with the verified thrust data to test its feasibility. The results indicate that thrust data from the force transducer and ECDS system are consistent with each other within the range of measurement error. Though the thrust data from the impulse thrust measurement system is a litter lower than that from the force transducer due to the axial momentum losses of the detonation jet, the impulse thrust measurement method is valid when applied to measure the averaged thrust of PDE. Analytical models of PDE are also discussed in this paper. The analytical thrust performance is higher than the experimental data due to ignoring the losses during the deflagration to detonation transition process. Effect of equivalence ratio on the engine thrust performance is investigated by utilizing the modified analytical model. Thrust reaches maximum at the equivalence ratio of about 1.1.

  5. Tiered analytics for purity assessment of macrocyclic peptides in drug discovery: Analytical consideration and method development.

    Science.gov (United States)

    Qian Cutrone, Jingfang Jenny; Huang, Xiaohua Stella; Kozlowski, Edward S; Bao, Ye; Wang, Yingzi; Poronsky, Christopher S; Drexler, Dieter M; Tymiak, Adrienne A

    2017-05-10

    Synthetic macrocyclic peptides with natural and unnatural amino acids have gained considerable attention from a number of pharmaceutical/biopharmaceutical companies in recent years as a promising approach to drug discovery, particularly for targets involving protein-protein or protein-peptide interactions. Analytical scientists charged with characterizing these leads face multiple challenges including dealing with a class of complex molecules with the potential for multiple isomers and variable charge states and no established standards for acceptable analytical characterization of materials used in drug discovery. In addition, due to the lack of intermediate purification during solid phase peptide synthesis, the final products usually contain a complex profile of impurities. In this paper, practical analytical strategies and methodologies were developed to address these challenges, including a tiered approach to assessing the purity of macrocyclic peptides at different stages of drug discovery. Our results also showed that successful progression and characterization of a new drug discovery modality benefited from active analytical engagement, focusing on fit-for-purpose analyses and leveraging a broad palette of analytical technologies and resources.

  6. Pesticides in honey: A review on chromatographic analytical methods.

    Science.gov (United States)

    Tette, Patrícia Amaral Souza; Rocha Guidi, Letícia; Glória, Maria Beatriz de Abreu; Fernandes, Christian

    2016-01-01

    Honey is a product of high consumption due to its nutritional and antimicrobial properties. However, residues of pesticides, used in plagues' treatment in the hive or in crop fields in the neighborhoods, can compromise its quality. Therefore, determination of these contaminants in honey is essential, since the use of pesticides has increased significantly in recent decades because of the growing demand for food production. Furthermore, pesticides in honey can be an indicator of environmental contamination. As the concentration of these compounds in honey is usually at trace levels and several pesticides can be found simultaneously, the use of highly sensitive and selective techniques is required. In this context, miniaturized sample preparation approaches and liquid or gas chromatography coupled to mass spectrometry became the most important analytical techniques. In this review we present and discuss recent studies dealing with pesticide determination in honey, focusing on sample preparation and separation/detection methods as well as application of the developed methods worldwide. Furthermore, trends and future perspectives are presented.

  7. Analytic-numerical method of determining the freezing front location

    Directory of Open Access Journals (Sweden)

    R. Grzymkowski

    2011-07-01

    Full Text Available Mathematical modeling of thermal processes combined with the reversible phase transitions of type: solid phase – liquid phase leads to formulation of the parabolic boundary problems with the moving boundary. Solution of such defined problem requires, most often, to use sophisticated numerical techniques and far advanced mathematical tools. Excellent illustration of the complexity of considered problems, as well as of the variety of approaches used for finding their solutions, gives the papers [1-4]. In the current paper, the authors present the, especially attractive from the engineer point of view, analytic-numerical method for finding the approximate solution of selected class of problems which can be reduced to the one-phase solidification problem of a plate with the unknown a priori, varying in time boundary of the region in which the solution is sought. Proposed method is based on the known formalism of initial expansion of the sought function describing the temperature field into the power series, some coefficients of which are determined with the aid of boundary conditions, and on the approximation of the function defining the location of freezing front with the broken line, parameters of which are numerically determined.

  8. Analytical one parameter method for PID motion controller settings

    NARCIS (Netherlands)

    Dijk, van J.; Aarts, R.G.K.M.

    2012-01-01

    In this paper analytical expressions for PID-controllers settings for electromechanical motion systems are presented. It will be shown that by an adequate frequency domain oriented parametrization, the parameters of a PID-controller are analytically dependent on one variable only, the cross-over fre

  9. Improved analytical method to study the cup anemometer performance

    Science.gov (United States)

    Pindado, Santiago; Ramos-Cenzano, Alvaro; Cubas, Javier

    2015-10-01

    The cup anemometer rotor aerodynamics is analytically studied based on the aerodynamics of a single cup. The effect of the rotation on the aerodynamic force is included in the analytical model, together with the displacement of the aerodynamic center during one turn of the cup. The model can be fitted to the testing results, indicating the presence of both the aforementioned effects.

  10. Are factor analytical techniques used appropriately in the validation of health status questionnaires?

    DEFF Research Database (Denmark)

    de Vet, Henrica C W; Adér, Herman J; Terwee, Caroline B

    2005-01-01

    Factor analysis is widely used to evaluate whether questionnaire items can be grouped into clusters representing different dimensions of the construct under study. This review focuses on the appropriate use of factor analysis. The Medical Outcomes Study Short Form-36 (SF-36) is used as an example...... of methods is crucial for correct interpretation of the results and verification of the conclusions. Our list of criteria may be useful for journal editors, reviewers and researchers who have to assess publications in which factor analysis is applied....... performed. Substantial shortcomings were found in the reporting and justification of the methods applied. In 15 of the 23 studies in which exploratory factor analysis was performed, confirmatory factor analysis would have been more appropriate. Cross-validation was rarely performed. Presentation...

  11. An analytical method for calculating torsional constants for arbitrary complicated thin-walled cross-sections

    Institute of Scientific and Technical Information of China (English)

    DU Baisong; GE Yaojun; ZHOU Zheng

    2007-01-01

    In this paper,an analytical method is proposed for calculating torsional constants for complicated thin-walled cross-sections with arbitrary closed or open rib stiffeners.This method uses the free torsional theory and the principle of virtual work to build goveming equilibrium equations involving unknown shear flows and twisting rate.After changing the form of the equations and combining these two unknowns into one,torsional function,which is a function of shear flow,shear modulus,and twisting rate,is included in the governing equations as only one of the unknowns.All the torsional functions can be easily obtained from these homogeneous linear equations,and torsional constants can be easily obtained from the torsional functions.The advantage of this method is that we can easily and directly obtain torsional constants from the torsional functions,rather than the more sophisticated shear flow and twisting rate calculations.Finally,a complicated thin-walled cross-section is given as a valid numerical example to verify the analytical method,which is much more accurate and simpler than the traditional finite element method.

  12. Simplex and duplex event-specific analytical methods for functional biotech maize.

    Science.gov (United States)

    Lee, Seong-Hun; Kim, Su-Jeong; Yi, Bu-Young

    2009-08-26

    Analytical methods are very important in the control of genetically modified organism (GMO) labeling systems or living modified organism (LMO) management for biotech crops. Event-specific primers and probes were developed for qualitative and quantitative analysis for biotech maize event 3272 and LY 038 on the basis of the 3' flanking regions, respectively. The qualitative primers confirmed the specificity by a single PCR product and sensitivity to 0.05% as a limit of detection (LOD). Simplex and duplex quantitative methods were also developed using TaqMan real-time PCR. One synthetic plasmid was constructed from two taxon-specific DNA sequences of maize and two event-specific 3' flanking DNA sequences of event 3272 and LY 038 as reference molecules. In-house validation of the quantitative methods was performed using six levels of mixing samples, from 0.1 to 10.0%. As a result, the biases from the true value and the relative deviations were all within the range of +/-30%. Limits of quantitation (LOQs) of the quantitative methods were all 0.1% for simplex real-time PCRs of event 3272 and LY 038 and 0.5% for duplex real-time PCR of LY 038. This study reports that event-specific analytical methods were applicable for qualitative and quantitative analysis for biotech maize event 3272 and LY 038.

  13. Comparative assessment of bioanalytical method validation guidelines for pharmaceutical industry.

    Science.gov (United States)

    Kadian, Naveen; Raju, Kanumuri Siva Rama; Rashid, Mamunur; Malik, Mohd Yaseen; Taneja, Isha; Wahajuddin, Muhammad

    2016-07-15

    The concepts, importance, and application of bioanalytical method validation have been discussed for a long time and validation of bioanalytical methods is widely accepted as pivotal before they are taken into routine use. United States Food and Drug Administration (USFDA) guidelines issued in 2001 have been referred for every guideline released ever since; may it be European Medical Agency (EMA) Europe, National Health Surveillance Agency (ANVISA) Brazil, Ministry of Health and Labour Welfare (MHLW) Japan or any other guideline in reference to bioanalytical method validation. After 12 years, USFDA released its new draft guideline for comments in 2013, which covers the latest parameters or topics encountered in bioanalytical method validation and approached towards the harmonization of bioanalytical method validation across the globe. Even though the regulatory agencies have general agreement, significant variations exist in acceptance criteria and methodology. The present review highlights the variations, similarities and comparison between bioanalytical method validation guidelines issued by major regulatory authorities worldwide. Additionally, other evaluation parameters such as matrix effect, incurred sample reanalysis including other stability aspects have been discussed to provide an ease of access for designing a bioanalytical method and its validation complying with the majority of drug authority guidelines.

  14. Validation of qualitative microbiological test methods

    NARCIS (Netherlands)

    IJzerman-Boon, Pieta C.; van den Heuvel, Edwin R.

    2015-01-01

    This paper considers a statistical model for the detection mechanism of qualitative microbiological test methods with a parameter for the detection proportion (the probability to detect a single organism) and a parameter for the false positive rate. It is demonstrated that the detection proportion a

  15. Optimization of the hydrofoil cascade and validation with quasi-analytical solution for hydraulic machinery

    Energy Technology Data Exchange (ETDEWEB)

    Frunza, T; Susan-Resiga, R [Department of Hydraulic Machinery, ' Politehnica' University of Timisoara Bv. Mihai Viteazu 1, RO-300222, Timisoara (Romania); Muntean, S; Bernad, S, E-mail: tfrunza@yahoo.co [Centre of Advanced Research in Engineering Sciences, Romanian Academy - Timisoara Branch, Bv. Mihai Viteazu 24, RO-300223, Timisoara (Romania)

    2010-08-15

    The paper presents the authors ongoing efforts to develop a robust and efficient numerical methodology, and the associated expert software, for analysis, design and optimization of hydrofoil cascades. We developed, so far, a Finite Element solver with streamfunction formulation for incompressible, inviscid and irrotational cascade flow, using a modern software infrastructure, and efficient implementation. Two test cases will be presented to evaluate the accuracy of our CASCADExpert code. In the first case, our code is tested for a thin hydrofoil cascade designed with the quasi-analytical approach. Second, the blade loading and thickness distributions obtain with our code from a given hydrofoil shape are used in an inverse design method. As a result, an optimized hydrofoil cascade is obtained. The pressure distribution on the original and optimized hydrofoil cascades is compared. We have applied the method in order to optimize the turbine and pump hydrofoil cascades, respectively. Consequently, a new method is developed in order to generate the optimized hydrofoil cascade geometry for hydraulic machinery.

  16. An analytical filter design method for guided wave phased arrays

    Science.gov (United States)

    Kwon, Hyu-Sang; Kim, Jin-Yeon

    2016-12-01

    This paper presents an analytical method for designing a spatial filter that processes the data from an array of two-dimensional guided wave transducers. An inverse problem is defined where the spatial filter coefficients are determined in such a way that a prescribed beam shape, i.e., a desired array output is best approximated in the least-squares sense. Taking advantage of the 2π-periodicity of the generated wave field, Fourier-series representation is used to derive closed-form expressions for the constituting matrix elements. Special cases in which the desired array output is an ideal delta function and a gate function are considered in a more explicit way. Numerical simulations are performed to examine the performance of the filters designed by the proposed method. It is shown that the proposed filters can significantly improve the beam quality in general. Most notable is that the proposed method does not compromise between the main lobe width and the sidelobe levels; i.e. a narrow main lobe and low sidelobes are simultaneously achieved. It is also shown that the proposed filter can compensate the effects of nonuniform directivity and sensitivity of array elements by explicitly taking these into account in the formulation. From an example of detecting two separate targets, how much the angular resolution can be improved as compared to the conventional delay-and-sum filter is quantitatively illustrated. Lamb wave based imaging of localized defects in an elastic plate using a circular array is also presented as an example of practical applications.

  17. An accelerated photo-magnetic imaging reconstruction algorithm based on an analytical forward solution and a fast Jacobian assembly method

    Science.gov (United States)

    Nouizi, F.; Erkol, H.; Luk, A.; Marks, M.; Unlu, M. B.; Gulsen, G.

    2016-10-01

    We previously introduced photo-magnetic imaging (PMI), an imaging technique that illuminates the medium under investigation with near-infrared light and measures the induced temperature increase using magnetic resonance thermometry (MRT). Using a multiphysics solver combining photon migration and heat diffusion, PMI models the spatiotemporal distribution of temperature variation and recovers high resolution optical absorption images using these temperature maps. In this paper, we present a new fast non-iterative reconstruction algorithm for PMI. This new algorithm uses analytic methods during the resolution of the forward problem and the assembly of the sensitivity matrix. We validate our new analytic-based algorithm with the first generation finite element method (FEM) based reconstruction algorithm previously developed by our team. The validation is performed using, first synthetic data and afterwards, real MRT measured temperature maps. Our new method accelerates the reconstruction process 30-fold when compared to a single iteration of the FEM-based algorithm.

  18. Validação de metodologia analítica para determinação de mercúrio total em amostras de urina por espectrometria de absorção atômica com geração de vapor frio (CV-AAS: estudo de caso Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS: case study

    Directory of Open Access Journals (Sweden)

    Sabine Neusatz Guilhen

    2010-01-01

    Full Text Available Mercury is a toxic metal used in a variety of substances over the course history. One of its more dubious uses is in dental amalgam restorations. It is possible to measure very small concentrations of this metal in the urine of exposed subjects by the cold vapor atomic absorption technique. The present work features the validation as an essential tool to confirm the suitability of the analytical method chosen to accomplish such determination. An initial analysis will be carried out in order to evaluate the environmental and occupational levels of exposure to mercury in 39 members of the auxiliary dental staff at public consulting rooms in the city of Araguaína (TO.

  19. ON A GENERALIZED TAYLOR THEOREM: A RATIONAL PROOF OF THE VALIDITY OF THE HOMOTOPY ANALYSIS METHOD

    Institute of Scientific and Technical Information of China (English)

    廖世俊

    2003-01-01

    A generalized Taylor series of a complex function was derived and some relatedtheorems about its convergence region were given. The generalized Taylor theorem can beapplied to greatly enlarge convergence regions of approximation series given by othertraditional techniques. The rigorous proof of the generalized Taylor theorem also provides uswith a rational base of the validity of a new kind of powerful analytic technique for nonlinearproblems, namely the homotopy analysis method.

  20. NIOSH Manual of Analytical Methods (third edition). Fourth supplement

    Energy Technology Data Exchange (ETDEWEB)

    1990-08-15

    The NIOSH Manual of Analytical Methods, 3rd edition, was updated for the following chemicals: allyl-glycidyl-ether, 2-aminopyridine, aspartame, bromine, chlorine, n-butylamine, n-butyl-glycidyl-ether, carbon-dioxide, carbon-monoxide, chlorinated-camphene, chloroacetaldehyde, p-chlorophenol, crotonaldehyde, 1,1-dimethylhydrazine, dinitro-o-cresol, ethyl-acetate, ethyl-formate, ethylenimine, sodium-fluoride, hydrogen-fluoride, cryolite, sodium-hexafluoroaluminate, formic-acid, hexachlorobutadiene, hydrogen-cyanide, hydrogen-sulfide, isopropyl-acetate, isopropyl-ether, isopropyl-glycidyl-ether, lead, lead-oxide, maleic-anhydride, methyl-acetate, methyl-acrylate, methyl-tert-butyl ether, methyl-cellosolve-acetate, methylcyclohexanol, 4,4'-methylenedianiline, monomethylaniline, monomethylhydrazine, nitric-oxide, p-nitroaniline, phenyl-ether, phenyl-ether-biphenyl mixture, phenyl-glycidyl-ether, phenylhydrazine, phosphine, ronnel, sulfuryl-fluoride, talc, tributyl-phosphate, 1,1,2-trichloro-1,2,2-trifluoroethane, trimellitic-anhydride, triorthocresyl-phosphate, triphenyl-phosphate, and vinyl-acetate.

  1. Validação em métodos cromatográficos e eletroforéticos Validation for chromatographic and electrophoretic methods

    Directory of Open Access Journals (Sweden)

    Marcelo Ribani

    2004-10-01

    Full Text Available The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the different Brazilian and international regulatory agencies.

  2. Validação de métodos analíticos na quantificação de comprimidos de Captopril - comparação de metodologias para um programa de garantia de qualidade - DOI: 10.4025/actascihealthsci.v26i2.1590 Validation of analytical methods for quantifying captopril in tablets – a comparison of methodologies for a quality control program - DOI: 10.4025/actascihealthsci.v26i2.1590

    Directory of Open Access Journals (Sweden)

    Graciette Matioli

    2004-04-01

    Full Text Available Atualmente, quando todos os caminhos levam à busca da qualidade total, torna-se indispensável conhecer perfeitamente cada fase de um processo produtivo. Neste caso, a validação é a ferramenta adequada para garantir a confiabilidade de instalação de um processo produtivo, de equipamento e, inclusive, da metodologia analítica. Dessa forma, o presente trabalho teve por objetivo analisar os principais aspectos da validação de métodos analíticos na quantificação do captopril. Foi realizada a validação e a comparação dos seguintes métodos: titulométrico por óxido-redução, espectrofotométrico por Folin-Ciocalteau e cromatográfico por cromatografia líquida de alta eficiência - CLAE. Os atributos de exatidão, precisão, linearidade, especificidade e robustez foram estudados para cada metodologia. Os resultados obtidos demonstraram que o método cromatográfico foi o mais adequado para as análises dos comprimidos de Captopril 25 mg, enquanto que os métodos espectrofotométrico e titulométrico demonstraram valores que satisfazem os critérios de aceitação, porém, com maior variabilidade e menor sensibilidade.Nowadays, when all approaches lead to the search for total quality, a thorough knowledge of every stage of a production process is vital. Validation is an appropriate tool to guarantee the reliabilities of: productive process installation, equipment and also analytical methodology. The aim of the present study was to analyze the main aspects of analytical methods validation for quantifying captopril. Validation and comparison of the following methods were carried out: titrimetric for oxide-reduction, spectrophotometry for Folin-Ciocalteau and high-efficiency liquid chromatography - HPLC. The attributes of accuracy, precision, linearity, specificity and robustness were studied for each methodology. The results show that the chromatographic method was the most suitable for Captopril 25 mg tablets evaluation, while the

  3. Evaluation of the quantitative performances of supercritical fluid chromatography: from method development to validation.

    Science.gov (United States)

    Dispas, Amandine; Lebrun, Pierre; Ziemons, Eric; Marini, Roland; Rozet, Eric; Hubert, Philippe

    2014-08-01

    Recently, the number of papers about SFC increased drastically but scientists did not truly focus their work on quantitative performances of this technique. In order to prove the potential of UHPSFC, the present work discussed about the different steps of the analytical life cycle of a method: from development to validation and application. Moreover, the UHPSFC quantitative performances were evaluated in comparison with UHPLC, which is the main technique used for quality control in the pharmaceutical industry and then could be considered as a reference. The methods were developed using Design Space strategy, leading to the optimization of robust method. In this context, when the Design Space optimization shows guarantee of quality, no more robustness study is required prior to the validation. Then, the methods were geometrically transferred in order to reduce the analysis time. The UHPSFC and UHPLC methods were validated based on the total error approach using accuracy profile. Even if UHPLC showed better precision and sensitivity, UHPSFC method is able to give accurate results in a dosing range larger than the 80-120% range required by the European Medicines Agency. Consequently, UHPSFC results are valid and could be used for the control of active substance in a finished pharmaceutical product. Finally, UHPSFC validated method was used to analyse real samples and gave similar results than the reference method (UHPLC).

  4. Fuzzy-logic based strategy for validation of multiplex methods: example with qualitative GMO assays.

    Science.gov (United States)

    Bellocchi, Gianni; Bertholet, Vincent; Hamels, Sandrine; Moens, W; Remacle, José; Van den Eede, Guy

    2010-02-01

    This paper illustrates the advantages that a fuzzy-based aggregation method could bring into the validation of a multiplex method for GMO detection (DualChip GMO kit, Eppendorf). Guidelines for validation of chemical, bio-chemical, pharmaceutical and genetic methods have been developed and ad hoc validation statistics are available and routinely used, for in-house and inter-laboratory testing, and decision-making. Fuzzy logic allows summarising the information obtained by independent validation statistics into one synthetic indicator of overall method performance. The microarray technology, introduced for simultaneous identification of multiple GMOs, poses specific validation issues (patterns of performance for a variety of GMOs at different concentrations). A fuzzy-based indicator for overall evaluation is illustrated in this paper, and applied to validation data for different genetically modified elements. Remarks were drawn on the analytical results. The fuzzy-logic based rules were shown to be applicable to improve interpretation of results and facilitate overall evaluation of the multiplex method.

  5. Analytical Validation of AmpliChip p53 Research Test for Archival Human Ovarian FFPE Sections.

    Directory of Open Access Journals (Sweden)

    Matthew J Marton

    Full Text Available The p53 tumor suppressor gene (TP53 is reported to be mutated in nearly half of all tumors and plays a central role in genome integrity. Detection of mutations in p53 can be accomplished by many assays, including the AmpliChip p53 Research Test. The AmpliChip p53 Research Test has been successfully used to determine p53 status in hematologic malignancies and fresh frozen solid tissues but there are few reports of using the assay with formalin fixed, paraffin-embedded (FFPE tissue. The objective of this study was to describe analytical performance characterization of the AmpliChip p53 Research Test to detect p53 mutations in genomic DNA isolated from archival FFPE human ovarian tumor tissues. Method correlation with sequencing showed 96% mutation-wise agreement and 99% chip-wise agreement. We furthermore observed 100% agreement (113/113 of the most prevalent TP53 mutations. Workflow reproducibility was 96.8% across 8 samples, with 2 operators, 2 reagent lots and 2 instruments. Section-to-section reproducibility was 100% for each sample across a 60 μm region of the FFPE block from ovarian tumors. These data indicate that the AmpliChip p53 Research Test is an accurate and reproducible method for detecting mutations in TP53 from archival FFPE human ovarian specimens.

  6. Development and Validation of a Learning Analytics Framework: Two Case Studies Using Support Vector Machines

    Science.gov (United States)

    Ifenthaler, Dirk; Widanapathirana, Chathuranga

    2014-01-01

    Interest in collecting and mining large sets of educational data on student background and performance to conduct research on learning and instruction has developed as an area generally referred to as learning analytics. Higher education leaders are recognizing the value of learning analytics for improving not only learning and teaching but also…

  7. Development of analytical methods for multiplex bio-assay with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Ornatsky, Olga I; Kinach, Robert; Bandura, Dmitry R; Lou, Xudong; Tanner, Scott D; Baranov, Vladimir I; Nitz, Mark; Winnik, Mitchell A

    2008-01-01

    Advances in the development of highly multiplexed bio-analytical assays with inductively coupled plasma mass spectrometry (ICP-MS) detection are discussed. Use of novel reagents specifically designed for immunological methods utilizing elemental analysis is presented. The major steps of method development, including selection of elements for tags, validation of tagged reagents, and examples of multiplexed assays, are considered in detail. The paper further describes experimental protocols for elemental tagging of antibodies, immunostaining of live and fixed human leukemia cells, and preparation of samples for ICP-MS analysis. Quantitative analysis of surface antigens on model cell lines using a cocktail of seven lanthanide labeled antibodies demonstrated high specificity and concordance with conventional immunophenotyping.

  8. Asymptotic analytical methods in fluid mechanics related to drag prediction

    Science.gov (United States)

    Inger, G. R.

    1975-01-01

    Some recent theoretical work of a purely analytical nature is described which promises to provide engineering predictions for the important drag-related phenomena of flow in the stall regime. This analytical work deals with rigorous asymptotic studies of the complete Navier-Stokes equations that govern the viscous flow around any aerodynamic body under conditions where boundary layer separation takes place from the body surface.

  9. Estimating Fuel Cycle Externalities: Analytical Methods and Issues, Report 2

    Energy Technology Data Exchange (ETDEWEB)

    Barnthouse, L.W.; Cada, G.F.; Cheng, M.-D.; Easterly, C.E.; Kroodsma, R.L.; Lee, R.; Shriner, D.S.; Tolbert, V.R.; Turner, R.S.

    1994-07-01

    of complex issues that also have not been fully addressed. This document contains two types of papers that seek to fill part of this void. Some of the papers describe analytical methods that can be applied to one of the five steps of the damage function approach. The other papers discuss some of the complex issues that arise in trying to estimate externalities. This report, the second in a series of eight reports, is part of a joint study by the U.S. Department of Energy (DOE) and the Commission of the European Communities (EC)* on the externalities of fuel cycles. Most of the papers in this report were originally written as working papers during the initial phases of this study. The papers provide descriptions of the (non-radiological) atmospheric dispersion modeling that the study uses; reviews much of the relevant literature on ecological and health effects, and on the economic valuation of those impacts; contains several papers on some of the more complex and contentious issues in estimating externalities; and describes a method for depicting the quality of scientific information that a study uses. The analytical methods and issues that this report discusses generally pertain to more than one of the fuel cycles, though not necessarily to all of them. The report is divided into six parts, each one focusing on a different subject area.

  10. Scattering From the Finite-Length, Dielectric Circular Cylinder. Part 2 - On the Validity of an Analytical Solution for Characterizing Backscattering from Tree Trunks at P-Band

    Science.gov (United States)

    2015-09-01

    flared base is expected to provide a closer emulation of trunk geometries encountered in nature. Only the 3-dB error lines for the analytical solution...On the Validity of an Analytical Solution for Characterizing Backscattering from Tree Trunks at P-Band by DaHan Liao...Validity of an Analytical Solution for Characterizing Backscattering from Tree Trunks at P-Band by DaHan Liao Sensors and Electron Devices

  11. Parametric design-based modal damped vibrational piezoelectric energy harvesters with arbitrary proof mass offset: Numerical and analytical validations

    Science.gov (United States)

    Lumentut, Mikail F.; Howard, Ian M.

    2016-02-01

    This paper focuses on the primary development of novel numerical and analytical techniques of the modal damped vibration energy harvesters with arbitrary proof mass offset. The key equations of electromechanical finite element discretisation using the extended Lagrangian principle are revealed and simplified to give matrix and scalar forms of the coupled system equations, indicating the most relevant numerical technique for the power harvester research. To evaluate the performance of the numerical study, the analytical closed-form boundary value equations have been developed using the extended Hamiltonian principle. The results from the electromechanical frequency response functions (EFRFs) derived from two theoretical studies show excellent agreement with experimental studies. The benefit of the numerical technique is in providing effective and quick predictions for analysing parametric designs and physical properties of piezoelectric materials. Although analytical technique provides a challenging process for analysing the complex smart structure, it shows complementary study for validating the numerical technique.

  12. An Analytic Method for the Kinematics and Dynamics of a Multiple-Backbone Continuum Robot

    Directory of Open Access Journals (Sweden)

    Bin He

    2013-01-01

    Full Text Available Continuum robots have been the subject of extensive research due to their potential use in a wide range of applications. In this paper, we propose a new continuum robot with three backbones, and provide a unified analytic method for the kinematics and dynamics of a multiple‐backbone continuum robot. The robot achieves actuation by independently pulling three backbones to carry out a bending motion of two‐degrees‐of‐freedom (DoF. A three‐dimensional CAD model of the robot is built and the kinematical equation is established on the basis of the Euler‐Bernoulli beam. The dynamical model of the continuum robot is constructed by using the Lagrange method. The simulation and the experiment’s validation results show the continuum robot can exactly bend into pre‐set angles in the two‐dimensional space (the maximum error is less than 5% of the robot length and can make a circular motion in three‐dimensional space. The results demonstrate that the proposed analytic method for the kinematics and dynamics of a continuum robot is feasible.

  13. Validation of three rapid screening methods for detection of verotoxin-producing Escherichia coli in foods : interlaboratory study

    NARCIS (Netherlands)

    Capps, K.L.; McLaughlin, E.M.; Murray, A.W.A.; Aldus, C.F.; Wyatt, G.M.; Peck, M.W.; Amerongen, van A.; Ariens, R.M.C.; Wichers, J.H.; Bayliss, C.L.; Wareing, D.R.A.; Bolton, F.J.

    2004-01-01

    An interlaboratory study was conducted for the validation of 3 methods for the detection of all verotoxin-producing Escherichia coli (VTEC) in foods. The methods were a multi-analyte 1-step lateral flow immunoassay (LFIA) for detection of E. coli O157 and verotoxin (VT); an enzyme-linked immunosorbe

  14. Desenvolvimento e validação de método analítico por cromatografia líquida de alta eficiência (CLAE para determinação de associação de ampicilinas em pó liofilizado para injeção Development and validation of analytical method for determination of an association of ampicillins in lyophilized powder for injection by HPLC

    Directory of Open Access Journals (Sweden)

    Ana Paola Prata Cione

    2010-01-01

    Full Text Available An analytical method has been developed and validated for the determination of an association of ampicillins in a lyophilized powder for injection by HPLC. The advantage of chromatographic method other than the microbiological one is that, it is possible to monitor precisely, out-of-specification results in quality control processes and also during stability studies, in which an association of ampicillins is present. The proposed HPLC method was developed by using forced degraded samples, in order to reach a selective analysis of ampicillins when in the presence of their degradation products. It was possible to detect benzatine and through indirect calculation, to determine the ampicillin sodium in the drug sample. The method showed to be selective, accurate, precise, robust and linear (from 45.92 to 36.04 μg mL-1 of total ampicillin and from 14.53 to 43.28 μg mL-1 of benzatine. The accuracy determined from recovery test, gave results in the range of 99.41% of total ampicillin to 100.31% of benzatine. Hence, it can be concluded that the proposed HPLC method is applicable for ampicillins determination.

  15. Validation of a screening method for rapid control of macrocyclic lactone mycotoxins in maize flour samples.

    Science.gov (United States)

    Zougagh, Mohammed; Téllez, Helena; Sánchez, Alberto; Chicharro, Manuel; Ríos, Angel

    2008-05-01

    A procedure for the analytical validation of a rapid supercritical fluid extraction amperometric screening method for controlling macrocyclic lactone mycotoxins in maize flour samples has been developed. The limit established by European legislation (0.2 mg kg(-1)), in reference to zearalenone (ZON) mycotoxin, was taken as the reference threshold to validate the proposed method. Natural ZON metabolites were also included in this study to characterize the final screening method. The objective was the reliable classification of samples as positive or negative samples. The cut-off level was fixed at a global concentration of mycotoxins of 0.17 mg kg(-1). An expanded unreliability zone between 0.16 and 0.23 mg kg(-1) characterized the screening method for classifying the samples. A set of 30 samples was used for the final demonstration of the reliability and usefulness of the method.

  16. Practical procedure for method validation in INAA- A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Petroni, Robson; Moreira, Edson G., E-mail: robsonpetroni@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    This paper describes the procedure employed by the Neutron Activation Laboratory at the Nuclear and Energy Research Institute (LAN, IPEN - CNEN/SP) for validation of Instrumental Neutron Activation Analysis (INAA) methods. According to recommendations of ISO/IEC 17025 the method performance characteristics (limit of detection, limit of quantification, trueness, repeatability, intermediate precision, reproducibility, selectivity, linearity and uncertainties budget) were outline in an easy, fast and convenient way. The paper presents step by step how to calculate the required method performance characteristics in a process of method validation, what are the procedures, adopted strategies and acceptance criteria for the results, that is, how to make a method validation in INAA. In order to exemplify the methodology applied, obtained results for the method validation of mass fraction determination of Co, Cr, Fe, Rb, Se and Zn in biological matrix samples, using an internal reference material of mussel tissue were presented. It was concluded that the methodology applied for validation of INAA methods is suitable, meeting all the requirements of ISO/IEC 17025, and thereby, generating satisfactory results for the studies carried at LAN, IPEN - CNEN/SP. (author)

  17. Semi-physiologic model validation and bioequivalence trials simulation to select the best analyte for acetylsalicylic acid.

    Science.gov (United States)

    Cuesta-Gragera, Ana; Navarro-Fontestad, Carmen; Mangas-Sanjuan, Victor; González-Álvarez, Isabel; García-Arieta, Alfredo; Trocóniz, Iñaki F; Casabó, Vicente G; Bermejo, Marival

    2015-07-10

    The objective of this paper is to apply a previously developed semi-physiologic pharmacokinetic model implemented in NONMEM to simulate bioequivalence trials (BE) of acetyl salicylic acid (ASA) in order to validate the model performance against ASA human experimental data. ASA is a drug with first-pass hepatic and intestinal metabolism following Michaelis-Menten kinetics that leads to the formation of two main metabolites in two generations (first and second generation metabolites). The first aim was to adapt the semi-physiological model for ASA in NOMMEN using ASA pharmacokinetic parameters from literature, showing its sequential metabolism. The second aim was to validate this model by comparing the results obtained in NONMEM simulations with published experimental data at a dose of 1000 mg. The validated model was used to simulate bioequivalence trials at 3 dose schemes (100, 1000 and 3000 mg) and with 6 test formulations with decreasing in vivo dissolution rate constants versus the reference formulation (kD 8-0.25 h (-1)). Finally, the third aim was to determine which analyte (parent drug, first generation or second generation metabolite) was more sensitive to changes in formulation performance. The validation results showed that the concentration-time curves obtained with the simulations reproduced closely the published experimental data, confirming model performance. The parent drug (ASA) was the analyte that showed to be more sensitive to the decrease in pharmaceutical quality, with the highest decrease in Cmax and AUC ratio between test and reference formulations.

  18. Numerical validation of the thermal quadrupoles method for a flow in a microchannel

    Directory of Open Access Journals (Sweden)

    Sabrine Mejri, Olivier Fudym, Jalila Sghaier, Ahmed Bellagi

    2016-01-01

    Full Text Available The main objective of this work is to investigate and validate the thermal quadrupole method, used in this paper as a semi-analytical method to solve the equations of a falling film in a heated microchannel studied experimentally. In the experimental section, we created a temperature gradient within the liquid, while monitoring the temperature using an infrared camera. Then, a numerical model is established and solved by the thermal quadrupole method. Finally, we conclude with a comparison between the experiments and the numerical study.

  19. Applied Nonlinear Dynamics Analytical, Computational, and Experimental Methods

    CERN Document Server

    Nayfeh, Ali H

    1995-01-01

    A unified and coherent treatment of analytical, computational and experimental techniques of nonlinear dynamics with numerous illustrative applications. Features a discourse on geometric concepts such as Poincaré maps. Discusses chaos, stability and bifurcation analysis for systems of differential and algebraic equations. Includes scores of examples to facilitate understanding.

  20. Thresholds for statistical and clinical significance in systematic reviews with meta-analytic methods

    DEFF Research Database (Denmark)

    Jakobsen, Janus Christian; Wetterslev, Jørn; Winkel, Per;

    2014-01-01

    BACKGROUND: Thresholds for statistical significance when assessing meta-analysis results are being insufficiently demonstrated by traditional 95% confidence intervals and P-values. Assessment of intervention effects in systematic reviews with meta-analysis deserves greater rigour. METHODS......: Methodologies for assessing statistical and clinical significance of intervention effects in systematic reviews were considered. Balancing simplicity and comprehensiveness, an operational procedure was developed, based mainly on The Cochrane Collaboration methodology and the Grading of Recommendations...... Assessment, Development, and Evaluation (GRADE) guidelines. RESULTS: We propose an eight-step procedure for better validation of meta-analytic results in systematic reviews (1) Obtain the 95% confidence intervals and the P-values from both fixed-effect and random-effects meta-analyses and report the most...

  1. Semi-analytical and numerical methods for computing transient waves in 2D acoustic / poroelastic stratified media

    CERN Document Server

    Lefeuve-Mesgouez, Gaëlle; Chiavassa, Guillaume; Lombard, Bruno

    2012-01-01

    Wave propagation in a stratified fluid / porous medium is studied here using analytical and numerical methods. The semi-analytical method is based on an exact stiffness matrix method coupled with a matrix conditioning procedure, preventing the occurrence of poorly conditioned numerical systems. Special attention is paid to calculating the Fourier integrals. The numerical method is based on a high order finite-difference time-domain scheme. Mesh refinement is applied near the interfaces to discretize the slow compressional diffusive wave predicted by Biot's theory. Lastly, an immersed interface method is used to discretize the boundary conditions. The numerical benchmarks are based on realistic soil parameters and on various degrees of hydraulic contact at the fluid / porous boundary. The time evolution of the acoustic pressure and the porous velocity is plotted in the case of one and four interfaces. The excellent level of agreement found to exist between the two approaches confirms the validity of both metho...

  2. Laser: a Tool for Optimization and Enhancement of Analytical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Preisler, Jan [Iowa State Univ., Ames, IA (United States)

    1997-01-01

    In this work, we use lasers to enhance possibilities of laser desorption methods and to optimize coating procedure for capillary electrophoresis (CE). We use several different instrumental arrangements to characterize matrix-assisted laser desorption (MALD) at atmospheric pressure and in vacuum. In imaging mode, 488-nm argon-ion laser beam is deflected by two acousto-optic deflectors to scan plumes desorbed at atmospheric pressure via absorption. All absorbing species, including neutral molecules, are monitored. Interesting features, e.g. differences between the initial plume and subsequent plumes desorbed from the same spot, or the formation of two plumes from one laser shot are observed. Total plume absorbance can be correlated with the acoustic signal generated by the desorption event. A model equation for the plume velocity as a function of time is proposed. Alternatively, the use of a static laser beam for observation enables reliable determination of plume velocities even when they are very high. Static scattering detection reveals negative influence of particle spallation on MS signal. Ion formation during MALD was monitored using 193-nm light to photodissociate a portion of insulin ion plume. These results define the optimal conditions for desorbing analytes from matrices, as opposed to achieving a compromise between efficient desorption and efficient ionization as is practiced in mass spectrometry. In CE experiment, we examined changes in a poly(ethylene oxide) (PEO) coating by continuously monitoring the electroosmotic flow (EOF) in a fused-silica capillary during electrophoresis. An imaging CCD camera was used to follow the motion of a fluorescent neutral marker zone along the length of the capillary excited by 488-nm Ar-ion laser. The PEO coating was shown to reduce the velocity of EOF by more than an order of magnitude compared to a bare capillary at pH 7.0. The coating protocol was important, especially at an intermediate pH of 7.7. The increase of p

  3. Analytic methods in assessment of optic nerve cupping.

    Science.gov (United States)

    Jindra, L F; Kuběna, T; Gaudino, R N

    2014-06-01

    The intent of this paper is to provide a systems-based analysis of the methods used to evaluate optic nerve cupping, identify potential flaws in these systems, and propose alternatives better to assess this anatomic quantity. Estimation of optic nerve cupping requires an analytic understanding of both the psychophysical as well as the mathematical bases inherent in this measure. When the (decimal-based) cup-to-disc ratio is used to quantitate optic nerve cupping, a one-dimensional, linear estimate is produced, which in turn is derived from two- or three-dimensional, non-linear physical quantities of area or volume, respectively. When extrapolating from volume, to area, to linear measures, due to the psychophysical constraints which limit this task, such a data-compressed estimate of optic nerve cupping may neither accurately reflect, nor correctly represent, the true amount of cupping actually present in the optic nerve head. This type of one-dimensional metric (when comparing calculations from two- or three-dimensional measures over a range of optic nerve cupping), appears to introduce errors which, while most pronounced earlier on in the disease progression, often overestimate the amount of relative cupping (percent cupping) present in a pathological process like glaucoma. The same systemic errors can also lead to overestimation of the progression in cupping, especially in optic nerves with low cup-to disc values. To provide clinically meaningful estimates of optic nerve cupping, the practitioner needs to be aware of psychophysical and mathematical limitations inherent in using a linear cup-to-disc ratio to estimate the amount of cupping observed in a physical structure like the optic disc. The resultant flaws introduced by observer extrapolation from three, to two, to one dimensions (volume, area, and linear); transposition from non-linear to linear quantities; and optical illusions, caused by factors like disc topology, morphology, and ametropia, can all

  4. Laser: a Tool for Optimization and Enhancement of Analytical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Preisler, Jan

    1997-01-01

    In this work, we use lasers to enhance possibilities of laser desorption methods and to optimize coating procedure for capillary electrophoresis (CE). We use several different instrumental arrangements to characterize matrix-assisted laser desorption (MALD) at atmospheric pressure and in vacuum. In imaging mode, 488-nm argon-ion laser beam is deflected by two acousto-optic deflectors to scan plumes desorbed at atmospheric pressure via absorption. All absorbing species, including neutral molecules, are monitored. Interesting features, e.g. differences between the initial plume and subsequent plumes desorbed from the same spot, or the formation of two plumes from one laser shot are observed. Total plume absorbance can be correlated with the acoustic signal generated by the desorption event. A model equation for the plume velocity as a function of time is proposed. Alternatively, the use of a static laser beam for observation enables reliable determination of plume velocities even when they are very high. Static scattering detection reveals negative influence of particle spallation on MS signal. Ion formation during MALD was monitored using 193-nm light to photodissociate a portion of insulin ion plume. These results define the optimal conditions for desorbing analytes from matrices, as opposed to achieving a compromise between efficient desorption and efficient ionization as is practiced in mass spectrometry. In CE experiment, we examined changes in a poly(ethylene oxide) (PEO) coating by continuously monitoring the electroosmotic flow (EOF) in a fused-silica capillary during electrophoresis. An imaging CCD camera was used to follow the motion of a fluorescent neutral marker zone along the length of the capillary excited by 488-nm Ar-ion laser. The PEO coating was shown to reduce the velocity of EOF by more than an order of magnitude compared to a bare capillary at pH 7.0. The coating protocol was important, especially at an intermediate pH of 7.7. The increase of p

  5. A new and consistent parameter for measuring the quality of multivariate analytical methods: Generalized analytical sensitivity.

    Science.gov (United States)

    Fragoso, Wallace; Allegrini, Franco; Olivieri, Alejandro C

    2016-08-24

    Generalized analytical sensitivity (γ) is proposed as a new figure of merit, which can be estimated from a multivariate calibration data set. It can be confidently applied to compare different calibration methodologies, and helps to solve literature inconsistencies on the relationship between classical sensitivity and prediction error. In contrast to the classical plain sensitivity, γ incorporates the noise properties in its definition, and its inverse is well correlated with root mean square errors of prediction in the presence of general noise structures. The proposal is supported by studying simulated and experimental first-order multivariate calibration systems with various models, namely multiple linear regression, principal component regression (PCR) and maximum likelihood PCR (MLPCR). The simulations included instrumental noise of different types: independently and identically distributed (iid), correlated (pink) and proportional noise, while the experimental data carried noise which is clearly non-iid.

  6. Hanford environmental analytical methods: Methods as of March 1990. Volume 3, Appendix A2-I

    Energy Technology Data Exchange (ETDEWEB)

    Goheen, S.C.; McCulloch, M.; Daniel, J.L.

    1993-05-01

    This paper from the analytical laboratories at Hanford describes the method used to measure pH of single-shell tank core samples. Sludge or solid samples are mixed with deionized water. The pH electrode used combines both a sensor and reference electrode in one unit. The meter amplifies the input signal from the electrode and displays the pH visually.

  7. Analytical modeling and experimental validation of a V-shape piezoelectric ultrasonic transducer

    Science.gov (United States)

    Li, Xiaoniu; Yao, Zhiyuan

    2016-07-01

    In this paper, an analytical model of a V-shape piezoelectric ultrasonic transducer is presented. The V-shape piezoelectric ultrasonic transducer has been widely applied to the piezoelectric actuator (ultrasonic motor), ultrasonic aided fabrication, sensor, and energy harvesting device. The V-shape piezoelectric ultrasonic transducer consists of two Langevin-type transducers connected together through a coupling point with a certain coupling angle. Considering the longitudinal and lateral movements of a single beam, the symmetrical and asymmetrical modals of the V-shape piezoelectric ultrasonic transducer are calculated. By using Hamilton-Lagrange equations, the electromechanical coupling model of the V-shape piezoelectric ultrasonic transducer is proposed. The influence of the coupling angle and cross-section on modal characteristics and electromechanical coupling coefficient are analyzed by the analytical model. A prototype of the V-shape piezoelectric ultrasonic transducer is fabricated, and the results of the experiments are in good agreement with the analytical model.

  8. Method validation for strobilurin fungicides in cereals and fruit

    DEFF Research Database (Denmark)

    Christensen, Hanne Bjerre; Granby, Kit

    2001-01-01

    Strobilurins are a new class of fungicides that are active against a broad spectrum of fungi. In the present work a GC method for analysis of strobilurin fungicides was validated. The method was based on extraction with ethyl acetate/cyclohexane, clean-up by gel permeation chromatography (GPC) an...

  9. Predictive validity of the Hand Arm Risk assessment Method (HARM)

    NARCIS (Netherlands)

    Douwes, M.; Boocock, M.; Coenen, P.; Heuvel, S. van den; Bosch, T.

    2014-01-01

    The Hand Arm Risk assessment Method (HARM) is a simplified risk assessment method for determining musculoskeletal symptoms to the arm, neck and/or shoulder posed by hand-arm tasks of the upper body. The purpose of this study was to evaluate the predictive validity of HARM using data collected from a

  10. Triangulation, Respondent Validation, and Democratic Participation in Mixed Methods Research

    Science.gov (United States)

    Torrance, Harry

    2012-01-01

    Over the past 10 years or so the "Field" of "Mixed Methods Research" (MMR) has increasingly been exerting itself as something separate, novel, and significant, with some advocates claiming paradigmatic status. Triangulation is an important component of mixed methods designs. Triangulation has its origins in attempts to validate research findings…

  11. A Numerical-analytic Method for Quickly Predicting Springback of Numerical Control Bending of Thin-walled Tube

    Institute of Scientific and Technical Information of China (English)

    Mei ZHAN; He YANG; Liang HUANG

    2006-01-01

    Springback is one of important factors influencing the forming quality of. numerical control(NC)bending of thin-walled tube. In this paper, a numerical-analytic method for springback angle prediction of the process was put forward. The method is based on springback angle model derived using analytic method and simulation results from three-dimensional(3D)rigid-plastic finite element method(FEM). The method is validated through comparison with experimental results. The features of the method are as follows:(1)The method is high in efficiency because it combines advantages of rigid-plastic FEM and analytic method.(2)The method is satisfactory in accuracy, since the field variables used in the model is resulting from 3D rigid-plastic FEM solution, and the effects both of axial force and strain neutral axis shift have been included.(3)Research on multi-factor effects can be carried out using the method due to its advantage inheriting from rigid-plastic FEM. The method described here is also of general significance to other bending processes.

  12. An analytic method for sensitivity analysis of complex systems

    Science.gov (United States)

    Zhu, Yueying; Wang, Qiuping Alexandre; Li, Wei; Cai, Xu

    2017-03-01

    Sensitivity analysis is concerned with understanding how the model output depends on uncertainties (variances) in inputs and identifying which inputs are important in contributing to the prediction imprecision. Uncertainty determination in output is the most crucial step in sensitivity analysis. In the present paper, an analytic expression, which can exactly evaluate the uncertainty in output as a function of the output's derivatives and inputs' central moments, is firstly deduced for general multivariate models with given relationship between output and inputs in terms of Taylor series expansion. A γ-order relative uncertainty for output, denoted by Rvγ, is introduced to quantify the contributions of input uncertainty of different orders. On this basis, it is shown that the widely used approximation considering the first order contribution from the variance of input variable can satisfactorily express the output uncertainty only when the input variance is very small or the input-output function is almost linear. Two applications of the analytic formula are performed to the power grid and economic systems where the sensitivities of both actual power output and Economic Order Quantity models are analyzed. The importance of each input variable in response to the model output is quantified by the analytic formula.

  13. Numerical Validation of the Delaunay Normalization and the Krylov-Bogoliubov-Mitropolsky Method

    Directory of Open Access Journals (Sweden)

    David Ortigosa

    2014-01-01

    Full Text Available A scalable second-order analytical orbit propagator programme based on modern and classical perturbation methods is being developed. As a first step in the validation and verification of part of our orbit propagator programme, we only consider the perturbation produced by zonal harmonic coefficients in the Earth’s gravity potential, so that it is possible to analyze the behaviour of the mathematical expressions involved in Delaunay normalization and the Krylov-Bogoliubov-Mitropolsky method in depth and determine their limits.

  14. Pressurised liquid extraction of flavonoids in onions. Method development and validation

    DEFF Research Database (Denmark)

    Søltoft, Malene; Christensen, J.H.; Nielsen, J.

    2009-01-01

    A rapid and reliable analytical method for quantification of flavonoids in onions was developed and validated. Five extraction methods were tested on freeze-dried onions and subsequently high performance liquid chromatography (HPLC) with UV detection was used for quantification of seven flavonoids....... The extraction efficiencies were lowest for the conventional water bath extraction compared to pressurized liquid extraction (PLE), ultrasonication, ultrasonic liquid processor, and microwave extraction, which yielded similar efficiencies. The reproducibility was in the same range (RSD: 1-11%) for all tested...

  15. Determination of Al in cake mix: Method validation and estimation of measurement uncertainty

    Science.gov (United States)

    Andrade, G.; Rocha, O.; Junqueira, R.

    2016-07-01

    An analytical method for the determination of Al in cake mix was developed. Acceptable values were obtained for the following parameters: linearity, detection limit - LOD (5.00 mg-kg-1) quantification limit - LOQ (12.5 mg-kg-1), the recovery assays values (between 91 and 102%), the relative standard deviation under repeatability and within-reproducibility conditions (<20.0%) and measurement uncertainty tests (<10.0%) The results of the validation process showed that the proposed method is fitness for purpose.

  16. VALIDATION OF CYCLAMATE ANALYSIS METHOD WITH SPECTROPHOTOMETRY AND TURBIDIMETRY

    Directory of Open Access Journals (Sweden)

    Regina Tutik Padmaningrum

    2016-04-01

    Full Text Available This research aims to validate methods of analysis by spectrophotometry and turbidimetry cyclamate in the sample drink mango-flavored jelly drink  by spectrophotometry with hypochlorite reagent, ultraviolet spectrophotometry (without reagent and turbidimetry. The object of research was the validity parameters spectrophotometric method were linearity, linear range, the limit of detection, limit of quantitation, precision, and accuracy. The calibration curve of standard solution of sodium cyclamate in the spectrophotometric method with hypochlorite reagent, UV spectrophotometry (without reagent, and turbidimetry are linear. Linear range each method respectively at a concentration were (211.36-747.08; (16.000-146.434; and (1.8521-6.1717 ppm. The detection limit of each method successively were 53.6028; 0.5833; and 0.2723 ppm. Limit of quantitation each method successively were 66.9948; 1.9443; and 0.8068 ppm. Spectrophotometric analysis method cyclamate with hypochlorite reagent had good precision and accuracy. Ultra violet  spectrophotometric analysis method of cyclamate have a good precision but the accuracy was not good. Turbidimetric methods  analysis of cyclamate had  precision and accuracy were not good. Keywords:   method validation, spectrophotometry, turbidimetry, cyclamate

  17. An analytical method for well-formed workflow/Petri net verification of classical soundness

    Directory of Open Access Journals (Sweden)

    Clempner Julio

    2014-12-01

    Full Text Available In this paper we consider workflow nets as dynamical systems governed by ordinary difference equations described by a particular class of Petri nets. Workflow nets are a formal model of business processes. Well-formed business processes correspond to sound workflow nets. Even if it seems necessary to require the soundness of workflow nets, there exist business processes with conditional behavior that will not necessarily satisfy the soundness property. In this sense, we propose an analytical method for showing that a workflow net satisfies the classical soundness property using a Petri net. To present our statement, we use Lyapunov stability theory to tackle the classical soundness verification problem for a class of dynamical systems described by Petri nets. This class of Petri nets allows a dynamical model representation that can be expressed in terms of difference equations. As a result, by applying Lyapunov theory, the classical soundness property for workflow nets is solved proving that the Petri net representation is stable. We show that a finite and non-blocking workflow net satisfies the sound property if and only if its corresponding PN is stable, i.e., given the incidence matrix A of the corresponding PN, there exists a Փ strictly positive m vector such that AՓ≤ 0. The key contribution of the paper is the analytical method itself that satisfies part of the definition of the classical soundness requirements. The method is designed for practical applications, guarantees that anomalies can be detected without domain knowledge, and can be easily implemented into existing commercial systems that do not support the verification of workflows. The validity of the proposed method is successfully demonstrated by application examples.

  18. Amphenicols stability in medicated feed – development and validation of liquid chromatography method

    Directory of Open Access Journals (Sweden)

    Pietro Wojciech Jerzy

    2014-12-01

    Full Text Available A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF and thiamphenicol (TAP in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3 on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm analytical column with UV (λ = 220 nm detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.

  19. Validación de un método de análisis para la determinación de hidrocarburos aromáticos policíclicos por cromatografía líquida de alta eficiencia en partículas PM10 Y PM2,5 Validation of an analytical method for the determination of polycyclic aromatic hydrocarbons by high efficiency liquid chromatography in PM10 and PM2, 5

    Directory of Open Access Journals (Sweden)

    Jorge Herrera Murillo

    2012-11-01

    Full Text Available Se validó un método analítico para la determinación de hidrocarburos aromáticos policíclicos presentes en partículas PM10 y PM 2,5 recolectadas en el aire mediante cromatografía líquida de alta resolución (CLAR. Los HPA incluidos en la metodología comprenden: Naftaleno, Acenaftileno, Fluoreno, Acenafteno, Fenantreno, Antraceno, Fluoranteno, Pireno, Benzo (aantraceno, Criseno, Benzo (bfluoranteno, Benzo (kfluoranteno, Benzo (apireno, Dibenzo (a,h antraceno, Benzo (g,h,iperileno y Indeno (1,2,3- C.D pireno. Para estos compuestos, los límites de detección y cuantificación estuvieron entre 0,02 y 0,1 mg/l utilizando un equipo marca Dionex modelo ICS- 3000, el cual consta de dos detectores en serie, un ultravioleta modelo VWD-1 y un detector de fluorescencia modelo RF-2000, permitiendo diferenciar las distintas señales de absorción y emisión para la debida identificación de los distintos compuestos. Para todos los compuestos analizados, el factor de recuperación resultó no ser significativamente diferente de uno y la repetibilidad y reproducibilidad resultó ser adecuada para un método analítico, especialmente para los HPA más ligeros.An analytical method for polycyclic aromatic hydrocarbons in PM10 and PM 2.5 par ticles collected from air by high performance liquid chromatography (HPLC was validated. The PAHs analyzed in the methodology include: Naphthalene, Acenaphthylene, Fluorene, Acenaphthene, Phenanthrene, Anthracene, fluoranthene,pyrene,Benzo(aanthracene,Chrysene, Benzo (bfluoranthene, Benzo (kfluoranthene, Benzo (apyrene Dibenzo (a, hanthracene, Benzo (g, h, iperylene and Indeno (1,2,3-CDpyrene. For these compounds, the detection limit and quantification limit were between 0,02 and 0,1 mg/l using a DIONEX ICS 3000 model cromatograph, that has two in serie detectors: UV/Vis and Fluorescense, separating the different absorption and emission signals for proper identification of individual compounds. For all the compounds

  20. Influence of the third energy level on the gain dynamics of EDFAs: analytical model and experimental validation.

    Science.gov (United States)

    De Varona, Omar; Steinke, Michael; Kracht, Dietmar; Neumann, Jörg; Wessels, Peter

    2016-10-31

    We report an analytical model and experimental validation of the temporal dynamics of 3-level system fiber amplifiers. The model predictions show a good agreement with the measured pump power to output power and the pump power to output phase transfer functions in an EDFA pumped at 976 nm, as well as with the typical literature values for the spontaneous lifetime of the involved energy levels. The measurements show a linear relation between the effective lifetime of the meta-stable level and the output power, and a filtering of the temperature-induced phase-shift due to the quantum defect at a sufficiently high frequency modulation.

  1. Development of analytical methods for polycyclic aromatic hydrocarbons (PAHs) in airborne particulates:A review

    Institute of Scientific and Technical Information of China (English)

    LIU Li-bin; LIU Yan; LIN Jin-ming; TANG Ning; HAYAKAWA Kazuichi; MAEDA Tsuneaki

    2007-01-01

    In the present work,the different sample collection, pretreatment and analytical methods for polycyclic aromatic hydrocarbons (PAHs) in airborne particulates is systematacially reviewed, and the applications of these pretreatment and analytical methods for PAHs are compared in detail. Some comments on the future expectation are also presented.

  2. Parametric validations of analytical lifetime estimates for radiation belt electron diffusion by whistler waves

    Directory of Open Access Journals (Sweden)

    A. V. Artemyev

    2013-04-01

    Full Text Available The lifetimes of electrons trapped in Earth's radiation belts can be calculated from quasi-linear pitch-angle diffusion by whistler-mode waves, provided that their frequency spectrum is broad enough and/or their average amplitude is not too large. Extensive comparisons between improved analytical lifetime estimates and full numerical calculations have been performed in a broad parameter range representative of a large part of the magnetosphere from L ~ 2 to 6. The effects of observed very oblique whistler waves are taken into account in both numerical and analytical calculations. Analytical lifetimes (and pitch-angle diffusion coefficients are found to be in good agreement with full numerical calculations based on CRRES and Cluster hiss and lightning-generated wave measurements inside the plasmasphere and Cluster lower-band chorus waves measurements in the outer belt for electron energies ranging from 100 keV to 5 MeV. Comparisons with lifetimes recently obtained from electron flux measurements on SAMPEX, SCATHA, SAC-C and DEMETER also show reasonable agreement.

  3. Evaluating water management strategies in watersheds by new hybrid Fuzzy Analytical Network Process (FANP) methods

    Science.gov (United States)

    RazaviToosi, S. L.; Samani, J. M. V.

    2016-03-01

    Watersheds are considered as hydrological units. Their other important aspects such as economic, social and environmental functions play crucial roles in sustainable development. The objective of this work is to develop methodologies to prioritize watersheds by considering different development strategies in environmental, social and economic sectors. This ranking could play a significant role in management to assign the most critical watersheds where by employing water management strategies, best condition changes are expected to be accomplished. Due to complex relations among different criteria, two new hybrid fuzzy ANP (Analytical Network Process) algorithms, fuzzy TOPSIS (Technique for Order Preference by Similarity to Ideal Solution) and fuzzy max-min set methods are used to provide more flexible and accurate decision model. Five watersheds in Iran named Oroomeyeh, Atrak, Sefidrood, Namak and Zayandehrood are considered as alternatives. Based on long term development goals, 38 water management strategies are defined as subcriteria in 10 clusters. The main advantage of the proposed methods is its ability to overcome uncertainty. This task is accomplished by using fuzzy numbers in all steps of the algorithms. To validate the proposed method, the final results were compared with those obtained from the ANP algorithm and the Spearman rank correlation coefficient is applied to find the similarity in the different ranking methods. Finally, the sensitivity analysis was conducted to investigate the influence of cluster weights on the final ranking.

  4. An experimental method for validating compressor valve vibration theory

    NARCIS (Netherlands)

    Habing, R.A.; Peters, M.C.A.M.

    2006-01-01

    This paper presents an experimental method for validating traditional compressor valve theory for unsteady flow conditions. Traditional valve theory considers the flow force acting on the plate and the flow rate as quasi-steady variables. These variables are related via semi-empirical coefficients w

  5. ePortfolios: The Method of Choice for Validation

    Science.gov (United States)

    Scott, Ken; Kim, Jichul

    2015-01-01

    Community colleges have long been institutions of higher education in the arenas of technical education and training, as well as preparing students for transfer to universities. While students are engaged in their student learning outcomes, projects, research, and community service, how have these students validated their work? One method of…

  6. A Rapid Gas Chromatography Method for Simultaneous Quantification of Ornidazole and Miconazole from Cream Formulations: Development, Validation and Application

    Directory of Open Access Journals (Sweden)

    Hetal M. Phatak

    2016-02-01

    Full Text Available Combination drug formulations are better in terms of effectiveness and hence are used many times for treatment of diseases. The physico-chemical properties of the different API used in a formulation have a significant impact in the development of a single method for the analysis of such drugs. In the current research a rapid analytical method employing GC-FID has been developed and validated for simultaneous quantification of the active ingredients Ornidazole and Miconazole from the cream formulation. The analytes were extracted from cream base and filtered. Adimethyl polysiloxane column is used for the separation of the analytes. The method involves simple temperature gradient and FID detection. Validation of the method showed response was a linear function of concentration in the range 50-150 µg mL−1 for both Ornidazole and Miconazole. The method was suitably validated and was found to be precise and robust, with recoveries for both the analytes being consistent and complete. The method has been successfully applied for the analysis of samples from marketed cream formulations.

  7. Development and Validation of a Path Analytic Model of Students' Performance in Chemistry.

    Science.gov (United States)

    Anamuah-Mensah, Jophus; And Others

    1987-01-01

    Reported the development and validation of an integrated model of performance on chemical concept-volumetric analysis. Model was tested on 265 chemistry students in eight schools.Results indicated that for subjects using algorithms without understanding, performance on volumetric analysis problems was not influenced by proportional reasoning…

  8. Analytical Quality by Design Approach in RP-HPLC Method Development for the Assay of Etofenamate in Dosage Forms.

    Science.gov (United States)

    Peraman, R; Bhadraya, K; Reddy, Y Padmanabha; Reddy, C Surayaprakash; Lokesh, T

    2015-01-01

    By considering the current regulatory requirement for an analytical method development, a reversed phase high performance liquid chromatographic method for routine analysis of etofenamate in dosage form has been optimized using analytical quality by design approach. Unlike routine approach, the present study was initiated with understanding of quality target product profile, analytical target profile and risk assessment for method variables that affect the method response. A liquid chromatography system equipped with a C18 column (250×4.6 mm, 5 μ), a binary pump and photodiode array detector were used in this work. The experiments were conducted based on plan by central composite design, which could save time, reagents and other resources. Sigma Tech software was used to plan and analyses the experimental observations and obtain quadratic process model. The process model was used for predictive solution for retention time. The predicted data from contour diagram for retention time were verified actually and it satisfied with actual experimental data. The optimized method was achieved at 1.2 ml/min flow rate of using mobile phase composition of methanol and 0.2% triethylamine in water at 85:15, % v/v, pH adjusted to 6.5. The method was validated and verified for targeted method performances, robustness and system suitability during method transfer.

  9. Chemical analysis of solid residue from liquid and solid fuel combustion: Method development and validation

    Energy Technology Data Exchange (ETDEWEB)

    Trkmic, M. [University of Zagreb, Faculty of Mechanical Engineering and Naval Architecturek Zagreb (Croatia); Curkovic, L. [University of Zagreb, Faculty of Chemical Engineering and Technology, Zagreb (Croatia); Asperger, D. [HEP-Proizvodnja, Thermal Power Plant Department, Zagreb (Croatia)

    2012-06-15

    This paper deals with the development and validation of methods for identifying the composition of solid residue after liquid and solid fuel combustion in thermal power plant furnaces. The methods were developed for energy dispersive X-ray fluorescence (EDXRF) spectrometer analysis. Due to the fuels used, the different composition and the location of creation of solid residue, it was necessary to develop two methods. The first method is used for identifying solid residue composition after fuel oil combustion (Method 1), while the second method is used for identifying solid residue composition after the combustion of solid fuels, i. e. coal (Method 2). Method calibration was performed on sets of 12 (Method 1) and 6 (Method 2) certified reference materials (CRM). CRMs and analysis test samples were prepared in pellet form using hydraulic press. For the purpose of method validation the linearity, accuracy, precision and specificity were determined, and the measurement uncertainty of methods for each analyte separately was assessed. The methods were applied in the analysis of real furnace residue samples. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. An analytic method for sensitivity analysis of complex systems

    CERN Document Server

    Zhu, Yueying; Li, Wei; Cai, Xu

    2016-01-01

    Sensitivity analysis is concerned with understanding how the model output depends on uncertainties (variances) in inputs and then identifies which inputs are important in contributing to the prediction imprecision. Uncertainty determination in output is the most crucial step in sensitivity analysis. In the present paper, an analytic expression, which can exactly evaluate the uncertainty in output as a function of the output's derivatives and inputs' central moments, is firstly deduced for general multivariate models with given relationship between output and inputs in terms of Taylor series expansion. A $\\gamma$-order relative uncertainty for output, denoted by $\\mathrm{R^{\\gamma}_v}$, is introduced to quantify the contributions of input uncertainty of different orders. On this basis, it is shown that the widely used approximation considering the first order contribution from the variance of input variable can satisfactorily express the output uncertainty only when the input variance is very small or the inpu...

  11. FREE VIBRATION OF ANISOTROPIC RECTANGULAR PLATES BY GENERAL ANALYTICAL METHOD

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    According to the differential equation for transverse displacement function of anisotropic rectangular thin plates in free vibration, a general analytical solution is established. This general solution, composed of the composite solutions of trigonometric function and hyperbolic function, can satisfy the problem of arbitrary boundary conditions along four edges. The algebraic polynomial with double sine series solutions can also satisfy the problem of boundary conditions at four corners. Consequently, this general solution can be used to solve the vibration problem of anisotropic rectangular plates with arbitrary boundaries accurately. The integral constants can be determined by boundary conditions of four edges and four corners. Each natural frequency and vibration mode can be solved by the determinate of coefficient matrix from the homogeneous linear algebraic equations equal to zero. For example, a composite symmetric angle ply laminated plate with four edges clamped has been calculated and discussed.

  12. Spectrophotometric validation of assay method for selected medicinal plant extracts

    OpenAIRE

    Matthew Arhewoh; Augustine O. Okhamafe

    2014-01-01

    Objective: To develop UV spectrophotometric assay validation methods for some selected medicinal plant extracts.Methods: Dried, powdered leaves of Annona muricata (AM) and Andrographis paniculata (AP) as well as seeds of Garcinia kola (GK) and Hunteria umbellata (HU) were separately subjected to maceration using distilled water. Different concentrations of the extracts were scanned spectrophotometrically to obtain wavelengths of maximum absorbance. The different extracts were then subjected t...

  13. Analytic Matrix Method for the Study of Propagation Characteristics of a Bent Planar Waveguide

    Institute of Scientific and Technical Information of China (English)

    LIU Qing; CAO Zhuang-Qi; SHEN Qi-Shun; DOU Xiao-Ming; CHEN Ying-Li

    2000-01-01

    An analytic matrix method is used to analyze and accurately calculate the propagation constant and bendinglosses of a bent planar waveguide. This method gives not only a dispersion equation with explicit physical insight,but also accurate complex propagation constants.

  14. Analytical Method for Designing Grating Compensated Dispersion-Managed Soliton Systems

    Institute of Scientific and Technical Information of China (English)

    Y.; H.; C.; Kwan; K.; Nakkeeran; P.; K.; A.; Wai

    2003-01-01

    We show a useful analytical method to design grating compensated dispersion-managed systems. Our method is in good agreement with the numerical results even in the presence of group delay ripples in the chirped fiber gratings.

  15. Preliminary Validation of High Performance Liquid Chromatography Method for Detection of Methyltestosterone Residue in Carp Muscle

    Institute of Scientific and Technical Information of China (English)

    JIANG Jie; LIN Hong; FU Xiaoting; LI Mingming

    2005-01-01

    The use of synthetic anabolic steroid methyltestosterone (MT) as growth promoter is prohibited in China. Validations of analytical methods for MT residue in food and the results obtained have become indispensable. The high performance liquid chromatography (HPLC) method for the detection of MT with liquid-liquid extraction by trichloromethanemethanol in carp muscle tissue was preliminarily validated with reference to the following parameters: recovery (accuracy)at the 1, 5 and 10 mgkg-1 level, between-run and within-run CV values (repeatability, also called relative standard deviation(RSD)) and limit of detection. The recoveries were above 80% and the between-run and within-run CV values below 10%for muscle tissue. The limit of detection was 0.05 mgkg-1.

  16. A Newly Improved Modified Method Development and Validation of Bromofenac Sodium Sesquihydrate in Bulk Drug Manufacturing

    Directory of Open Access Journals (Sweden)

    Sunil Kumar Yelamanchi V

    2016-10-01

    Full Text Available The main objective of this study was to develop a simple, efficient, specific, precise and accurate newly improved modified Reverse Phase High Performance Liquid Chromatographic Purity (or Related substance method for bromofenac sodium sesquihydrate active pharmaceuticals ingredient dosage form. Validation of analytical method is the confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are fulfilled as per ICH, USP, BP or any other suitable regulatory guidelines. The Reverse Phase High Performance Liquid Chromatographic Gradient method was developed by utilizing Waters Symmetry C8, 150x4.6mm, 3.5µm on Waters 2487 series Liquid Chromatograph. The retention time of bromofenac sodium sesquihydrate was found to be 5.973minutes. Considering all the results of validation parameters simplicity of the method and the cost effectiveness of the overall procedure, it is possible to conclude that the developed method can be suitable for the regular quality control determination of bromofenac sodium sesquihydrate in bulk as well as pharmaceutical dosage form.The developed Reverse Phase High Performance Liquid Chromatographic Purity (or Related substance method for bromofenac sodium sesquihydrate active pharmaceuticals ingredient method was validated with respect to System Suitability , linearity, , precision ,Range, Ruggedness, Test Solution and Mobile phase stability ,Robustness..

  17. Five-point Element Scheme of Finite Analytic Method for Unsteady Groundwater Flow

    Institute of Scientific and Technical Information of China (English)

    Xiang Bo; Mi Xiao; Ji Changming; Luo Qingsong

    2007-01-01

    In order to improve the finite analytic method's adaptability for irregular unit, by using coordinates rotation technique this paper establishes a five-point element scheme of finite analytic method. It not only solves unsteady groundwater flow equation but also gives the boundary condition. This method can be used to calculate the three typical questions of groundwater. By compared with predecessor's computed result, the result of this method is more satisfactory.

  18. Analytical methods for the determination of carbon tetrachloride in soils.

    Energy Technology Data Exchange (ETDEWEB)

    Alvarado, J. S.; Spokas, K.; Taylor, J.

    1999-06-01

    Improved methods for the determination of carbon tetrachloride are described. These methods incorporate purge-and-trap concentration of heated dry samples, an improved methanol extraction procedure, and headspace sampling. The methods minimize sample pretreatment, accomplish solvent substitution, and save time. The methanol extraction and headspace sampling procedures improved the method detection limits and yielded better sensitivity, good recoveries, and good performance. Optimization parameters are shown. Results obtained with these techniques are compared for soil samples from contaminated sites.

  19. Analysis of plasticizers in PVC medical devices: Performance comparison of eight analytical methods.

    Science.gov (United States)

    Bernard, L; Bourdeaux, D; Pereira, B; Azaroual, N; Barthélémy, C; Breysse, C; Chennell, P; Cueff, R; Dine, T; Eljezi, T; Feutry, F; Genay, S; Kambia, N; Lecoeur, M; Masse, M; Odou, P; Radaniel, T; Simon, N; Vaccher, C; Verlhac, C; Yessad, M; Décaudin, B; Sautou, V

    2017-01-01

    A wide variety of medical devices (MDs) used in hospitals are made of flexible plasticized polyvinylchloride (PVC). Different plasticizers are present in variable amounts in the PVC matrix of the devices and can leach out into the infused solutions and may enter into contact with the patients. The ARMED(1) project aims to assess the migration of these plasticizers from medical devices and therefore the level of exposure in patients. For the first task of the project, eight methods were developed to directly detect and quantify the plasticizers in the PVC matrix of the MDs. We compared the overall performances of the analytical methods using standardized and validated criteria in order to provide the scientific community with the guidance and the technical specifications of each method for the intended application. We have shown that routine rapid screening could be performed directly on the MDs using the FTIR technique, with cost-effective analyses. LC techniques may also be used, but with limits and only with individual quantification of the main plasticizers expected in the PVC matrix. GC techniques, especially GC-MS, are both more specific and more sensitive than other techniques. NMR is a robust and specific technique to precisely discriminate all plasticizers in a MD but is limited by its cost and its low ability to detect and quantify plasticizer contamination, e.g. by DEHP. All these results have been confirmed by a real test, called the " blind test " carried out on 10 MD samples.

  20. Dimensionless Maps for the Validity of Analytical Ground Heat Transfer Models for GSHP Applications

    Directory of Open Access Journals (Sweden)

    Paolo Conti

    2016-10-01

    Full Text Available This article provides plain and handy expressions to decide the most suitable analytical model for the thermal analysis of the ground source in vertical ground-coupled heat pump applications. We perform a comprehensive dimensionless analysis of the reciprocal deviation among the classical infinite, finite, linear and cylindrical heat source models in purely conductive media. Besides, we complete the framework of possible boreholes model with the “hollow” finite cylindrical heat source solution, still lacking in the literature. Analytical expressions are effective tools for both design and performance assessment: they are able to provide practical and general indications on the thermal behavior of the ground with an advantageous tradeoff between calculation efforts and solution accuracy. This notwithstanding, their applicability to any specific case is always subjected to the coherence of the model assumptions, also in terms of length and time scales, with the specific case of interest. We propose several dimensionless criteria to evaluate when one model is practically equivalent to another one and handy maps that can be used for both design and performance analysis. Finally, we found that the finite line source represents the most suitable model for borehole heat exchangers (BHEs, as it is applicable to a wide range of space and time scales, practically providing the same results of more complex models.

  1. Potential data used for validation of concentration statistics obtained using analytical model for conservative transport in an estuary

    Science.gov (United States)

    Galesic, Morena; Andricevic, Roko; Divic, Vladimir; Mateus, Marcos; Pinto, Ligia

    2016-04-01

    Coastal areas worldwide are important and sensitive ecosystems. Rivers are considered to be one of the most influential hydrological pathways for the waterborne transport and therefore estuaries are critical areas for a pollution hazard. To describe that hazard, the risk of exceeding the allowed concentration values of the pollution substance in such environment is often used. The analytical model calculates concentration statistics directly from the fundamental advective-diffusion equation for the case of continuous, steady conservative transport with the dominant stream flow mean velocity such is the case of low tide estuaries. Similar analytical models were previously proposed in atmosphere (Sullivan, 2004) and in groundwater (Andricevic, 2008). Knowing the main velocity and initial mass coming from the river, this kind of approach enables one a direct prediction of one-point concentration probability density function (pdf) which is then used to define the risk of exceeding the allowed concentration for certain water body. In this work we investigate how different data can be used for validation of the developed analytical model for conservative transport in an estuary. Two different types of measurement are being conducted at the local river Zrnovnica near city of Split, one measuring velocity and the other measuring salinity and temperature. Velocity data are used as an input to a numerical random walk particle tracking model to calculate the concentration moments. The salinity data are used as inverse proxy substance, hence the concentration moments are calculated directly from the inverse measured values. The results are highly affected by the scale effect, as the analytical model is developed at the point, while both numerical and measured values are smoothed over the grid size and over the sampling volume, respectively. However, the measured salinity, as concentration proxy, proved more resemblance to the concentration moment's shape, while numerical model

  2. Analytical method for assessing potential dermal exposure to captan, using whole body dosimetry, in small vegetable production units in Argentina.

    Science.gov (United States)

    Hughes, Enrique A; Zalts, Anita; Ojeda, Javier J; Flores, Andrea P; Glass, Richard C; Montserrat, Javier M

    2006-09-01

    An analytical method has been developed that can be used to determine the potential dermal exposure (PDE) of workers to the pesticide captan in small-scale horticultural production units. The methodology is based on the whole body dosimetry technique, using a cotton coverall and cotton gloves as sampling media, with protective clothing worn beneath the cotton media to protect the operator. The quantitative determination of captan was done by gas chromatography-electron capture detector (GC-ECD), with the analytical method validated by measuring limits of detection and quantification, linear ranges, sample recovery and precision. Special emphasis is placed on factors that affected the stability of captan during chromatographic determination. The data generated for potential dermal exposure are presented separately for mixing/loading and application activities. These data are compared with values obtained with visible tracers using a similar field technique. Margin of safety (MOS) values are also calculated for the agricultural procedures studied.

  3. Determination of paraquat and diquat: LC-MS method optimization and validation.

    Science.gov (United States)

    Pizzutti, Ionara R; Vela, Giovana M E; de Kok, André; Scholten, Jos M; Dias, Jonatan V; Cardoso, Carmem D; Concenço, Germani; Vivian, Rafael

    2016-10-15

    This study describes the optimization and single-laboratory validation of a single residue method for determination of two bipyridylium herbicides, paraquat and diquat, in cowpeas by UPLC-MS/MS in a total run time of 9.3min. The method is based on extraction with an acidified methanol-water mixture. Different extraction parameters (extraction solvent composition, temperature, sample extract filtration, and pre-treatment of the laboratory sample) were evaluated in order to optimize the extraction method efficiency. Isotopically labeled internal standards, Paraquat-D6 and Diquat-D4, were used and added to the test portions prior to extraction. The method validation was performed by analyzing spiked samples at three concentrations (10, 20 and 50μgkg(-1)), with seven replicates (n=7) for each concentration. Linearity (r(2)) of analytical curves, accuracy (trueness as recovery % and precision as RSD%), instrument and method limits of detection and quantification (LOD and LOQ) and matrix effects were determined. Average recoveries obtained for diquat were between 77 and 85% with RSD values ⩽20%, for all spike levels studied. On the other hand, paraquat showed average recoveries between 68 and 103% with RSDs in the range 14.4-25.4%. The method LOQ was 10 and 20μgkg(-1) for diquat and paraquat, respectively. The matrix effect was significant for both pesticides. Consequently, matrix-matched calibration standards and using isotopically labeled (IL) analogues as internal standards for the target analytes are required for application in routine analysis. The validated method was successfully applied for cowpea samples obtained from various field studies.

  4. A Validated HPLC-DAD Method for Simultaneous Determination of Etodolac and Pantoprazole in Rat Plasma

    Directory of Open Access Journals (Sweden)

    Ali S. Abdelhameed

    2014-01-01

    Full Text Available A simple, sensitive, and accurate HPLC-DAD method has been developed and validated for the simultaneous determination of pantoprazole and etodolac in rat plasma as a tool for therapeutic drug monitoring. Optimal chromatographic separation of the analytes was achieved on a Waters Symmetry C18 column using a mobile phase that consisted of phosphate buffer pH~4.0 as eluent A and acetonitrile as eluent B in a ratio of A : B, 55 : 45 v/v for 6 min, pumped isocratically at a flow rate of 0.8 mL min−1. The eluted analytes were monitored using photodiode array detector set to quantify samples at 254 nm. The method was linear with r2=0.9999 for PTZ and r2=0.9995 for ETD at a concentration range of 0.1–15 and 5–50 μgmL−1 for PTZ and ETD, respectively. The limits of detection were found to be 0.033 and 0.918 μgmL−1 for PTZ and ETD, respectively. The method was statistically validated for linearity, accuracy, precision, and selectivity following the International Conference for Harmonization (ICH guidelines. The reproducibility of the method was reliable with the intra- and interday precision (% RSD <7.76% for PTZ and <7.58 % for ETD.

  5. Method development and validation for dieckol in the standardization of phlorotannin preparations

    Directory of Open Access Journals (Sweden)

    Jiyoung Kim

    2016-03-01

    Full Text Available Abstract Phlorotannins are reported to have diverse biological properties. However, no analytical methods for the standardization of phlorotannin preparations have been reported. Herein, we developed and validated an analytical method for the determination of dieckol in phlorotannin extracts (PRT using high-performance liquid chromatography (HPLC. The optimum HPLC conditions consisted of a Supelco Discovery C18 column stationary phase, a mobile phase (A: 15 % HPLC grade methanol in deionized water, B: methanol, UV detection at 230 nm, and a flow rate of 0.7 mL/min. The optimized chromatographic conditions were validated and exhibited good specificity and linearity (R 2 > 0.9994–1.0000. The recoveries were in the range of 100.9–102.3 %. The method had good intermediate (%RSD 1.2 and intra-day (%RSD 0.4–1.7 assay precisions. This HPLC method had good accuracy and quality in the determination of dieckol in PRT.

  6. Development and method validation for the determination of nitroimidazole residues in salmon, tilapia and shrimp muscle.

    Science.gov (United States)

    Watson, Lynn; Potter, Ross; MacNeil, James D; Murphy, Cory

    2014-01-01

    The use of nitroimidazoles in aquacultured fish has been banned in many countries due to the suspected mutagenic and carcinogenic effects of these compounds. In response to the need to conduct residue testing of these compounds in fish, a simple, rapid, and sensitive method was developed and validated that is suitable for regulatory monitoring of nitroimidazole residues and their hydroxy metabolites in fish muscle tissue. Following solvent extraction of homogenized tissue and clean-up using a C18 SPE cartridge, analyses were conducted by ultra-performance UPLC-MS/MS. A precursor ion and two product ions were monitored for each of the parent compounds and metabolites included in the method. The validated method has an analytical range from 1 to 50 ng/g in the representative species (tilapia, salmon, and shrimp), with an LOD and LOQ ranging from 0.07 to 1.0 nglg and 0.21 to 3.0 nglg, respectively, depending on the analyte. Recoveries ranged from 81 to 124% and repeatability was between 4 and 17%. HorRat values were within typical limits of acceptability for a single laboratory. Working standards were stable for 12 months, extracts were stable for 5 days, and tissues for 2 months under appropriate storage conditions. This method was determined to be suitable for routine use for screening, quantification, and confirmation of nitroimidazole residues in a residue monitoring program for fish with regulatory oversight.

  7. Gas chromatographic validated method for quantification of ayurvedic polyherbal formulation

    Directory of Open Access Journals (Sweden)

    Navdeep Saini

    2015-01-01

    Full Text Available A new gas chromatographic-flame ionization detector (GC-FID method was developed for quantification of ayurvedic polyherbal formulation. The GC-FID method was found highly accurate, sensitive, simple and precise. This method was validated as per international conference on harmonization (ICH guidelines. Experimental work was performed by nonpolar capillary column (Zb-5, 5%-Phenyl-95%-dimethylpolysiloxane. Film thickness of capillary column (Zb-5 was (0.25 μm and length 30 m × 0.25 mm i.d. The temperature of the oven, injector and detector were 200, 210 and 280°C respectively. Data processing system was applied to obtain data. The standards and test samples were prepared in absolute ethanol. The principle constituents t-Anethol, d-Limonene, cuminaldehyde and thymol were found in ayurvedic polyherbal formulation. The ICH validation parameters for the proposed procedure, recovery (limit 98.85-100.76%, precision (<1.00%, limits of detection, limits of quantification and linearity (r2 = 0.995 ± 0.002 were observed under acceptance limit. Validation results were statistically calculated. The result shows that method is selective and reproducible for quantification of ayurvedic polyherbal formulation. The presented GC method can be applied for the routine analysis of principle constituents as well as ayurvedic polyherbal formulation.

  8. In-house validation and quality control of real-time PCR methods for GMO detection: a practical approach.

    Science.gov (United States)

    Ciabatti, I; Froiio, A; Gatto, F; Amaddeo, D; Marchesi, U

    2006-01-01

    GMO detection and quantification methods in the EU are mainly based on real-time PCR. The analytical methods in use must be validated, first on an intra-laboratory scale and through a collaborative trial thereafter. Since a consensual protocol for intra-laboratory validation of real-time PCR methods is lacking, we provide a practical approach for the in-house validation of quantitative real-time PCR methods, establishing acceptability criteria and quality controls for PCR runs. Parameters such as limit of detection, limit of quantification, precision, trueness, linear dynamic range, PCR efficiency, robustness and specificity are considered. The protocol is sufficiently detailed to be directly applicable, increases the reliability of results and their harmonization among different laboratories, and represents a necessary preliminary step before proceeding to a time-consuming and costly full validation study.

  9. Analysis of Carbamate Pesticides: Validation of Semi-Volatile Analysis by HPLC-MS/MS by EPA Method MS666

    Energy Technology Data Exchange (ETDEWEB)

    Owens, J; Koester, C

    2008-05-14

    The Environmental Protection Agency's (EPA) Region 5 Chicago Regional Laboratory (CRL) developed a method for analysis of aldicarb, bromadiolone, carbofuran, oxamyl, and methomyl in water by high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS), titled Method EPA MS666. This draft standard operating procedure (SOP) was distributed to multiple EPA laboratories and to Lawrence Livermore National Laboratory, which was tasked to serve as a reference laboratory for EPA's Environmental Reference Laboratory Network (ERLN) and to develop and validate analytical procedures. The primary objective of this study was to validate and verify the analytical procedures described in MS666 for analysis of carbamate pesticides in aqueous samples. The gathered data from this validation study will be used to: (1) demonstrate analytical method performance; (2) generate quality control acceptance criteria; and (3) revise the SOP to provide a validated method that would be available for use during a homeland security event. The data contained in this report will be compiled, by EPA CRL, with data generated by other EPA Regional laboratories so that performance metrics of Method EPA MS666 can be determined.

  10. Development and Validation of an HPLC Method for the Analysis of Sirolimus in Drug Products

    Directory of Open Access Journals (Sweden)

    Hadi Valizadeh

    2012-05-01

    Full Text Available Purpose: The aim of this study was to develop a simple, rapid and sensitive reverse phase high performance liquid chromatography (RP-HPLC method for quantification of sirolimus (SRL in pharmaceutical dosage forms. Methods: The chromatographic system employs isocratic elution using a Knauer- C18, 5 mm, 4.6 × 150 mm. Mobile phase consisting of acetonitril and ammonium acetate buffer set at flow rate 1.5 ml/min. The analyte was detected and quantified at 278nm using ultraviolet detector. The method was validated as per ICH guidelines. Results: The standard curve was found to have a linear relationship (r2 > 0.99 over the analytical range of 125–2000ng/ml. For all quality control (QC standards in intraday and interday assay, accuracy and precision range were -0.96 to 6.30 and 0.86 to 13.74 respectively, demonstrating the precision and accuracy over the analytical range. Samples were stable during preparation and analysis procedure. Conclusion: Therefore the rapid and sensitive developed method can be used for the routine analysis of sirolimus such as dissolution and stability assays of pre- and post-marketed dosage forms.

  11. An experimental-analytical method to study steady spray combustion.

    Science.gov (United States)

    Bracco, F. V.

    1973-01-01

    Description of a method for determining the local parameters of the gas mixture resulting from the combustion of sprayed fuel in a gaseous oxidizer. The method is based on the measurement of local static pressures in the gas mixture and does not require the knowledge of the droplet distribution function, drag, and vaporization characteristics. A set of equations with substituted local pressure values is used for calculations. Application of the method is demonstrated on a liquid oxygen-ethanol rocket fuel.

  12. Team mental models: techniques, methods, and analytic approaches.

    Science.gov (United States)

    Langan-Fox, J; Code, S; Langfield-Smith, K

    2000-01-01

    Effective team functioning requires the existence of a shared or team mental model among members of a team. However, the best method for measuring team mental models is unclear. Methods reported vary in terms of how mental model content is elicited and analyzed or represented. We review the strengths and weaknesses of vatrious methods that have been used to elicit, represent, and analyze individual and team mental models and provide recommendations for method selection and development. We describe the nature of mental models and review techniques that have been used to elicit and represent them. We focus on a case study on selecting a method to examine team mental models in industry. The processes involved in the selection and development of an appropriate method for eliciting, representing, and analyzing team mental models are described. The criteria for method selection were (a) applicability to the problem under investigation; (b) practical considerations - suitability for collecting data from the targeted research sample; and (c) theoretical rationale - the assumption that associative networks in memory are a basis for the development of mental models. We provide an evaluation of the method matched to the research problem and make recommendations for future research. The practical applications of this research include the provision of a technique for analyzing team mental models in organizations, the development of methods and processes for eliciting a mental model from research participants in their normal work environment, and a survey of available methodologies for mental model research.

  13. Determination of chloramphenicol in bovine urine, meat and shrimp by GC-MS. Method validation according to Commission Decision 2002/657/EC

    NARCIS (Netherlands)

    Rossum HJ van; Kootstra PR; Sterk SS; ARO

    2004-01-01

    This report describes the validation of the quantification and the identification of an analytical method for the determination of low concentrations (0.1-1.0 micro g/kg) of chloramphenicol in samples of urine, shrimps and meat. The validation study was based on the criteria described in Decision 20

  14. 75 FR 49930 - Stakeholder Meeting Regarding Re-Evaluation of Currently Approved Total Coliform Analytical Methods

    Science.gov (United States)

    2010-08-16

    ... AGENCY Stakeholder Meeting Regarding Re-Evaluation of Currently Approved Total Coliform Analytical... technical dialogue with stakeholders regarding re-evaluation of currently approved Total Coliform Rule (TCR) analytical methods. At these meetings, stakeholders will be given an opportunity to discuss...

  15. Hybrid analytic-numeric calculation method for light through a bounded planar dielectric

    NARCIS (Netherlands)

    Nicolau, J.B.; Groesen, van E.

    2005-01-01

    We present a hybrid analytic-numeric method to calculate the transmission and reflection of light that is fluxed into a bounded complicated optical structure surrounded by air. The solution is obtained by numerical calculations inside a square containing the structure and by analytical calculations

  16. Application of an analytical method for solution of thermal hydraulic conservation equations

    Energy Technology Data Exchange (ETDEWEB)

    Fakory, M.R. [Simulation, Systems & Services Technologies Company (S3 Technologies), Columbia, MD (United States)

    1995-09-01

    An analytical method has been developed and applied for solution of two-phase flow conservation equations. The test results for application of the model for simulation of BWR transients are presented and compared with the results obtained from application of the explicit method for integration of conservation equations. The test results show that with application of the analytical method for integration of conservation equations, the Courant limitation associated with explicit Euler method of integration was eliminated. The results obtained from application of the analytical method (with large time steps) agreed well with the results obtained from application of explicit method of integration (with time steps smaller than the size imposed by Courant limitation). The results demonstrate that application of the analytical approach significantly improves the numerical stability and computational efficiency.

  17. Improved chiral SFC screening for analytical method development.

    Science.gov (United States)

    Schafer, Wes; Chandrasekaran, Tilak; Pirzada, Zainab; Zhang, Chaowei; Gong, Xiaoyi; Biba, Mirlinda; Regalado, Erik L; Welch, Christopher J

    2013-11-01

    In this study we describe the evaluation of a recently developed supercritical fluid chromatography (SFC) instrument for automated chiral SFC method development. The greatly improved gradient dwell volume and liquid flow control of the new instrument in combination with the use of shorter columns containing smaller stationary phase particles affords chiral SFC method development that is faster and more universal than previous systems.

  18. An Analytical Method for Measuring Competence in Project Management

    Science.gov (United States)

    González-Marcos, Ana; Alba-Elías, Fernando; Ordieres-Meré, Joaquín

    2016-01-01

    The goal of this paper is to present a competence assessment method in project management that is based on participants' performance and value creation. It seeks to close an existing gap in competence assessment in higher education. The proposed method relies on information and communication technology (ICT) tools and combines Project Management…

  19. Methods for Geometric Data Validation of 3d City Models

    Science.gov (United States)

    Wagner, D.; Alam, N.; Wewetzer, M.; Pries, M.; Coors, V.

    2015-12-01

    Geometric quality of 3D city models is crucial for data analysis and simulation tasks, which are part of modern applications of the data (e.g. potential heating energy consumption of city quarters, solar potential, etc.). Geometric quality in these contexts is however a different concept as it is for 2D maps. In the latter case, aspects such as positional or temporal accuracy and correctness represent typical quality metrics of the data. They are defined in ISO 19157 and should be mentioned as part of the metadata. 3D data has a far wider range of aspects which influence their quality, plus the idea of quality itself is application dependent. Thus, concepts for definition of quality are needed, including methods to validate these definitions. Quality on this sense means internal validation and detection of inconsistent or wrong geometry according to a predefined set of rules. A useful starting point would be to have correct geometry in accordance with ISO 19107. A valid solid should consist of planar faces which touch their neighbours exclusively in defined corner points and edges. No gaps between them are allowed, and the whole feature must be 2-manifold. In this paper, we present methods to validate common geometric requirements for building geometry. Different checks based on several algorithms have been implemented to validate a set of rules derived from the solid definition mentioned above (e.g. water tightness of the solid or planarity of its polygons), as they were developed for the software tool CityDoctor. The method of each check is specified, with a special focus on the discussion of tolerance values where they are necessary. The checks include polygon level checks to validate the correctness of each polygon, i.e. closeness of the bounding linear ring and planarity. On the solid level, which is only validated if the polygons have passed validation, correct polygon orientation is checked, after self-intersections outside of defined corner points and edges

  20. Validation study of a rapid ELISA for detection of aflatoxin in corn. Performance Tested Method 050901.

    Science.gov (United States)

    Lupo, Anthony; Roebuck, Chris; Dutcher, Monica; Kennedy, Justina; Abouzied, Mohamed

    2010-01-01

    Neogen Corp. developed the Veratox aflatoxin test kit for the detection of total aflatoxin. The purpose of this study was to validate the method under the requirements of the AOAC Research Institute Performance Tested Methods (PTM) program. There are several AOAC Official Methods for total aflatoxin detection in corn (994.08, 990.33, 979.18, 993.17, 990.32, 993.16, 991.31, and 990.74), varying between rapid and analytical-based methods and one rapid method that has been performance tested by the AOAC Research Institute (PTM 030701). However, the widely used reference method is AOAC Official Method 994.08, which is an HPLC method and is referred to as the reference method in this paper. Although considered the reference method, the HPLC procedure is complicated and requires the investment of both expensive equipment and a highly skilled technician. A rapid (e.g., ELISA) test kit to be validated by the AOAC Research Institute is needed.

  1. Manual of analytical methods for the Industrial Hygiene Chemistry Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Greulich, K.A.; Gray, C.E. (comp.)

    1991-08-01

    This Manual is compiled from techniques used in the Industrial Hygiene Chemistry Laboratory of Sandia National Laboratories in Albuquerque, New Mexico. The procedures are similar to those used in other laboratories devoted to industrial hygiene practices. Some of the methods are standard; some, modified to suit our needs; and still others, developed at Sandia. The authors have attempted to present all methods in a simple and concise manner but in sufficient detail to make them readily usable. It is not to be inferred that these methods are universal for any type of sample, but they have been found very reliable for the types of samples mentioned.

  2. Base flow separation: A comparison of analytical and mass balance methods

    Science.gov (United States)

    Lott, Darline A.; Stewart, Mark T.

    2016-04-01

    Base flow is the ground water contribution to stream flow. Many activities, such as water resource management, calibrating hydrological and climate models, and studies of basin hydrology, require good estimates of base flow. The base flow component of stream flow is usually determined by separating a stream hydrograph into two components, base flow and runoff. Analytical methods, mathematical functions or algorithms used to calculate base flow directly from discharge, are the most widely used base flow separation methods and are often used without calibration to basin or gage-specific parameters other than basin area. In this study, six analytical methods are compared to a mass balance method, the conductivity mass-balance (CMB) method. The base flow index (BFI) values for 35 stream gages are obtained from each of the seven methods with each gage having at least two consecutive years of specific conductance data and 30 years of continuous discharge data. BFI is cumulative base flow divided by cumulative total discharge over the period of record of analysis. The BFI value is dimensionless, and always varies from 0 to 1. Areas of basins used in this study range from 27 km2 to 68,117 km2. BFI was first determined for the uncalibrated analytical methods. The parameters of each analytical method were then calibrated to produce BFI values as close to the CMB derived BFI values as possible. One of the methods, the power function (aQb + cQ) method, is inherently calibrated and was not recalibrated. The uncalibrated analytical methods have an average correlation coefficient of 0.43 when compared to CMB-derived values, and an average correlation coefficient of 0.93 when calibrated with the CMB method. Once calibrated, the analytical methods can closely reproduce the base flow values of a mass balance method. Therefore, it is recommended that analytical methods be calibrated against tracer or mass balance methods.

  3. Elasto-plastic strain analysis by a semi-analytical method

    Indian Academy of Sciences (India)

    Debabrata Das; Prasanta Sahoo; Kashinath Saha

    2008-08-01

    The aim of this paper is to develop a simulation model of large deformation problems following a semi-analytical method, incorporating the complications of geometric and material non-linearity in the formulation. The solution algorithm is based on the method of energy principle in structural mechanics, as applicable for conservative systems. A one-dimensional solid circular bar problem has been solved in post-elastic range assuming linear elastic, linear strain hardening material behaviour. Type of loading includes uniform uniaxial loading and gravity loading due to body force, whereas the geometry of the bar is considered to be non-uniformly taper. Results are validated successfully with benchmark solution and some new results have also been reported. The location of initiation of elasto-plastic front and its growth are found to be functions of geometry of the bar and loading conditions. Some indicative results have been presented for static and dynamic problems and the solution methodology developed for one-dimension has been extended to the elasto-plastic analysis of two-dimensional strain field problems of a rotating disk.

  4. Size-selective poorly soluble particulate reference materials for evaluation of quantitative analytical methods.

    Science.gov (United States)

    Stefaniak, Aleksandr B; Turk, Gregory C; Dickerson, Robert M; Hoover, Mark D

    2008-07-01

    Owing to the absence of readily available certified particulate reference materials (RMs), most analytical methods used to determine particulate contaminant levels in workplace or other environments are validated using solution RMs, which do not assess the robustness of the digestion step for all forms and sizes of particles in a sample. A library of particulate RMs having a range of chemical forms and particle sizes is needed to support a shift in method evaluation strategies to include both solution and particulate RMs. In support of creating this library, we characterized bulk and physically size separated fractions of beryllium oxide (BeO) particles recovered from the machining fluid sludge of an industrial ceramic products grinding operation. Particles were large agglomerates of compact, crystalline BeO primary particles having diameters on the order of several micrometers. As expected, the particle surface area was independent of sieve size, with a range from 3.61 m(2)/g (53-63-microm fraction) to 4.82 m(2)/g (355-600-microm fraction). The density was near the theoretical value (3.01 g/cm(3)). The data support more detailed characterization of the sludge materials for use as size-selective RMs. This work illustrates an approach that can be used to develop RMs that are difficult to digest.

  5. Validated HPTLC method for the simultaneous determination of cinnarizine and dimenhydrinate in their combined dosage form

    Directory of Open Access Journals (Sweden)

    Dina S. El-Kafrawy

    2016-02-01

    Full Text Available A simple, rapid and selective high performance thin layer chromatography (HPTLC method was developed for the simultaneous determination of cinnarizine (CNZ and dimenhydrinate (DMH in pure form and in their combined dosage form. Reviewing the literature revealed that there are no reports for the use of TLC for the assay of this mixture. Effective separation was achieved using Fluka HPTLC aluminum sheets of silica gel 60 F254 using chloroform–n-hexane–methanol (8.5:0.8:0.7, by volume as mobile phase, followed by densitometric measurement of CNZ and DMH spots at 254 and 279 nm, respectively. The reliability and analytical performance of the proposed HPTLC method were statistically validated with respect to linearity, ranges, precision, accuracy, selectivity, robustness and detection and quantification limits. Calibration curves were linear in the ranges of 50–400 and 50–500 ng/spot for CNZ and DMH, respectively with correlation coefficients >0.9998. The limits of detection were 8.1 and 8.0 ng/spot for CNZ and DMH respectively. The validated HPTLC method was applied to the simultaneous analysis of CNZ and DMH in laboratory-prepared tablets. Both analytes were successfully quantified with good recovery values, and no interference was encountered from the inactive ingredients.

  6. 40 CFR 136.6 - Method modifications and analytical requirements.

    Science.gov (United States)

    2010-07-01

    ..., oil and grease, total suspended solids, total phenolics, turbidity, chemical oxygen demand, and..., an analyst may not modify an approved method if the modification would result in measurement of...

  7. Analytical method for promoting process capability of shock absorption steel

    Institute of Scientific and Technical Information of China (English)

    2003-01-01

    Mechanical properties and low cycle fatigue are two factors that must be considered in developing new type steel for shock absorption. Process capability and process control are significant factors in achieving the purpose of research and development programs. Often-used evaluation methods failed to measure process yield and process centering; so this paper uses Taguchi loss function as basis to establish an evaluation method and the steps for assessing the quality of mechanical properties and process control of an iron and steel manufacturer. The establishment of this method can serve the research and development and manufacturing industry and lay a foundation in enhancing its process control ability to select better manufacturing processes that are more reliable than decision making by using the other commonly used methods.

  8. Analytical Evaluation of Beam Deformation Problem Using Approximate Methods

    DEFF Research Database (Denmark)

    Barari, Amin; Kimiaeifar, A.; Domairry, G.

    2010-01-01

    The beam deformation equation has very wide applications in structural engineering. As a differential equation, it has its own problem concerning existence, uniqueness and methods of solutions. Often, original forms of governing differential equations used in engineering problems are simplified...

  9. Validating the JobFit system functional assessment method

    Energy Technology Data Exchange (ETDEWEB)

    Jenny Legge; Robin Burgess-Limerick

    2007-05-15

    Workplace injuries are costing the Australian coal mining industry and its communities $410 Million a year. This ACARP study aims to meet those demands by developing a safe, reliable and valid pre-employment functional assessment tool. All JobFit System Pre-Employment Functional Assessments (PEFAs) consist of a musculoskeletal screen, balance test, aerobic fitness test and job-specific postural tolerances and material handling tasks. The results of each component are compared to the applicant's job demands and an overall PEFA score between 1 and 4 is given with 1 being the better score. The reliability study and validity study were conducted concurrently. The reliability study examined test-retest, intra-tester and inter-tester reliability of the JobFit System Functional Assessment Method. Overall, good to excellent reliability was found, which was sufficient to be used for comparison with injury data for determining the validity of the assessment. The overall assessment score and material handling tasks had the greatest reliability. The validity study compared the assessment results of 336 records from a Queensland underground and open cut coal mine with their injury records. A predictive relationship was found between PEFA score and the risk of a back/trunk/shoulder injury from manual handling. An association was also found between PEFA score of 1 and increased length of employment. Lower aerobic fitness test results had an inverse relationship with injury rates. The study found that underground workers, regardless of PEFA score, were more likely to have an injury when compared to other departments. No relationship was found between age and risk of injury. These results confirm the validity of the JobFit System Functional Assessment method.

  10. Development, optimization and validation of a sub-minute analytical enantioselective high performance liquid chromatographic separation for a folic acid precursor in normal phase mode.

    Science.gov (United States)

    Frühauf, Doris; Juza, Markus

    2012-12-21

    A sub-minute enantioselective normal phase high performance liquid chromatographic (HPLC) method for the analysis of a chiral precursor molecule employed frequently in folic acid syntheses was developed, optimized and successfully validated according to ICH-guidelines. It could be shown that ultra-high performance chromatography (UHPLC) can give significant advantages compared to traditional HPLC not only in reversed phase HPLC, but also for enantioselective separations in normal phase mode. Novel 3 μm-particle sizes allow developing analytical chromatographic methods completely resolving two enantiomers in the shortest time possible while preserving high efficiency and low detection limits. By offering increased resolution, sensitivity and speed, enantioselective UHPLC (eUHPLC) improves sample throughput, productivity and provides considerably faster access to information on enantiomeric purity also under non-aqueous conditions.

  11. Method validation and analysis of nine dithiocarbamates in fruits and vegetables by LC-MS/MS

    DEFF Research Database (Denmark)

    Schmidt, Bjørn; Christensen, Hanne Bjerre; Petersen, Annette

    2013-01-01

    An analytical method for separation and quantitative determination of nine dithiocarbamates (DTCs) in fruits and vegetables by using LC-MS/MS was developed, validated and applied to samples purchased in local supermarkets. The nine DTCs were ziram, ferbam, thiram, maneb, zineb, nabam, metiram......, mancozeb and propineb. Validation parameters of mean recovery for two matrices at two concentration levels, relative repeatability (RSDr), relative within-laboratory reproducibility (RSDR) and LOD were obtained for the nine DTCs. The results from the analysis of fruits and vegetables served as the basis...... the various DTCs in the LC-MS/MS analysis was lacking. The exposure and risk assessment showed that only for maneb in the case of apples and apple juice, the acute reference dose was exceeded for infants in the United Kingdom and for children in Germany, respectively....

  12. Bayesian structural equation modeling method for hierarchical model validation

    Energy Technology Data Exchange (ETDEWEB)

    Jiang Xiaomo [Department of Civil and Environmental Engineering, Vanderbilt University, Box 1831-B, Nashville, TN 37235 (United States)], E-mail: xiaomo.jiang@vanderbilt.edu; Mahadevan, Sankaran [Department of Civil and Environmental Engineering, Vanderbilt University, Box 1831-B, Nashville, TN 37235 (United States)], E-mail: sankaran.mahadevan@vanderbilt.edu

    2009-04-15

    A building block approach to model validation may proceed through various levels, such as material to component to subsystem to system, comparing model predictions with experimental observations at each level. Usually, experimental data becomes scarce as one proceeds from lower to higher levels. This paper presents a structural equation modeling approach to make use of the lower-level data for higher-level model validation under uncertainty, integrating several components: lower-level data, higher-level data, computational model, and latent variables. The method proposed in this paper uses latent variables to model two sets of relationships, namely, the computational model to system-level data, and lower-level data to system-level data. A Bayesian network with Markov chain Monte Carlo simulation is applied to represent the two relationships and to estimate the influencing factors between them. Bayesian hypothesis testing is employed to quantify the confidence in the predictive model at the system level, and the role of lower-level data in the model validation assessment at the system level. The proposed methodology is implemented for hierarchical assessment of three validation problems, using discrete observations and time-series data.

  13. Prognostics of Power Electronics, Methods and Validation Experiments

    Science.gov (United States)

    Kulkarni, Chetan S.; Celaya, Jose R.; Biswas, Gautam; Goebel, Kai

    2012-01-01

    Abstract Failure of electronic devices is a concern for future electric aircrafts that will see an increase of electronics to drive and control safety-critical equipment throughout the aircraft. As a result, investigation of precursors to failure in electronics and prediction of remaining life of electronic components is of key importance. DC-DC power converters are power electronics systems employed typically as sourcing elements for avionics equipment. Current research efforts in prognostics for these power systems focuses on the identification of failure mechanisms and the development of accelerated aging methodologies and systems to accelerate the aging process of test devices, while continuously measuring key electrical and thermal parameters. Preliminary model-based prognostics algorithms have been developed making use of empirical degradation models and physics-inspired degradation model with focus on key components like electrolytic capacitors and power MOSFETs (metal-oxide-semiconductor-field-effect-transistor). This paper presents current results on the development of validation methods for prognostics algorithms of power electrolytic capacitors. Particularly, in the use of accelerated aging systems for algorithm validation. Validation of prognostics algorithms present difficulties in practice due to the lack of run-to-failure experiments in deployed systems. By using accelerated experiments, we circumvent this problem in order to define initial validation activities.

  14. Comparison of analytical and predictive methods for water, protein, fat, sugar, and gross energy in marine mammal milk.

    Science.gov (United States)

    Oftedal, O T; Eisert, R; Barrell, G K

    2014-01-01

    sugar methods for total sugar-appear likely to produce substantial error in marine mammal milks. It is important that alternative analytical methods be properly validated against a reference method before being used, especially for mammalian milks that differ greatly from cow milk in analyte characteristics and concentrations.

  15. Analytical method for promoting process capability of shock absorption steel

    Institute of Scientific and Technical Information of China (English)

    SUNGWen-Pei; SHIHMing-Hsiang; CHENKuen-Suan

    2003-01-01

    Mechanical properties and low cycle fatigue are two factors that must be considered in developin gnew type steel for shock absorption. Process capability and process control are significant factors in achieving the purpose of research and development programs. Often-used evaluation methods failed to measure processyield and process centering ; so this paper uses Taguchi loss function as basis to establish an evaluation methodand the steps for assessing the quality of mechanical properties and process control of an iron and steel manu-facturer. The establishment of this method can serve the research and development and manufacturing industry and lay a foundation in enhancing its process control ability to select better manufacturing processes that are more reliable than decision making by using the other commonly used methods.

  16. Analytical Model Analysis Of Distributed Cooperative Spectrum Sensing Method

    Directory of Open Access Journals (Sweden)

    Ravi Prakash Shukla

    2012-05-01

    Full Text Available Spectrum sensing is a key function of cognitive radio to prevent the harmful interference with licensed users and identify the available spectrum for improving the spectrum’s utilization. Various methods for spectrum sensing control, such as deciding which sensors should perform sensing simultaneously and finding the appropriate trade-off between probability of misdetection and false alarm rate, are described. However, detection performance in practice is often compromised with multipath fading, shadowing and receiver uncertainty issues. To mitigate the impact of these issues, cooperative spectrum sensing has been shown to be an effective method to improve the detection performance by exploiting spatial diversity.

  17. An Analytical Method of Identifying Biased Test Items.

    Science.gov (United States)

    Plake, Barbara S.; Hoover, H. D.

    1979-01-01

    A follow-up technique is needed to identify items contributing to items-by-groups interaction when using an ANOVA procedure to examine a test for biased items. The method described includes distribution theory for assessing level of significance and is sensitive to items at all difficulty levels. (Author/GSK)

  18. Analytic method for solitary solutions of some partial differential equations

    Energy Technology Data Exchange (ETDEWEB)

    Ugurlu, Yavuz [Firat University, Department of Mathematics, 23119 Elazig (Turkey); Kaya, Dogan [Firat University, Department of Mathematics, 23119 Elazig (Turkey)], E-mail: dkaya@firat.edu.tr

    2007-10-22

    In this Letter by considering an improved tanh function method, we found some exact solutions of the clannish random walker's parabolic equation, the modified Korteweg-de Vries (KdV) equation, and the Sharma-Tasso-Olver (STO) equation with its fission and fusion, the Jaulent-Miodek equation.

  19. Study on Fluorescence Analytical Method of Micro Th in Pu

    Institute of Scientific and Technical Information of China (English)

    QIAN; Hong-juan; ZHANG; Li-hua; LIU; Huan-liang; FAN; De-jun

    2013-01-01

    As one of impurities,Th is needed to be determined for control quality of Pu product.Due to the high radioactivity and fatal toxicity of Pu,it is very difficult to measure the micro Th in Pu product.It is necessary to develop a sensitive method for determining the micro Th in Pu under the described harsh condition.

  20. OWL-based reasoning methods for validating archetypes.

    Science.gov (United States)

    Menárguez-Tortosa, Marcos; Fernández-Breis, Jesualdo Tomás

    2013-04-01

    Some modern Electronic Healthcare Record (EHR) architectures and standards are based on the dual model-based architecture, which defines two conceptual levels: reference model and archetype model. Such architectures represent EHR domain knowledge by means of archetypes, which are considered by many researchers to play a fundamental role for the achievement of semantic interoperability in healthcare. Consequently, formal methods for validating archetypes are necessary. In recent years, there has been an increasing interest in exploring how semantic web technologies in general, and ontologies in particular, can facilitate the representation and management of archetypes, including binding to terminologies, but no solution based on such technologies has been provided to date to validate archetypes. Our approach represents archetypes by means of OWL ontologies. This permits to combine the two levels of the dual model-based architecture in one modeling framework which can also integrate terminologies available in OWL format. The validation method consists of reasoning on those ontologies to find modeling errors in archetypes: incorrect restrictions over the reference model, non-conformant archetype specializations and inconsistent terminological bindings. The archetypes available in the repositories supported by the openEHR Foundation and the NHS Connecting for Health Program, which are the two largest publicly available ones, have been analyzed with our validation method. For such purpose, we have implemented a software tool called Archeck. Our results show that around 1/5 of archetype specializations contain modeling errors, the most common mistakes being related to coded terms and terminological bindings. The analysis of each repository reveals that different patterns of errors are found in both repositories. This result reinforces the need for making serious efforts in improving archetype design processes.

  1. Temperature based validation of the analytical model for the estimation of the amount of heat generated during friction stir welding

    Directory of Open Access Journals (Sweden)

    Milčić Dragan S.

    2012-01-01

    Full Text Available Friction stir welding is a solid-state welding technique that utilizes thermomechanical influence of the rotating welding tool on parent material resulting in a monolith joint - weld. On the contact of welding tool and parent material, significant stirring and deformation of parent material appears, and during this process, mechanical energy is partially transformed into heat. Generated heat affects the temperature of the welding tool and parent material, thus the proposed analytical model for the estimation of the amount of generated heat can be verified by temperature: analytically determined heat is used for numerical estimation of the temperature of parent material and this temperature is compared to the experimentally determined temperature. Numerical solution is estimated using the finite difference method - explicit scheme with adaptive grid, considering influence of temperature on material's conductivity, contact conditions between welding tool and parent material, material flow around welding tool, etc. The analytical model shows that 60-100% of mechanical power given to the welding tool is transformed into heat, while the comparison of results shows the maximal relative difference between the analytical and experimental temperature of about 10%.

  2. On the gravitational signature of zonal flows in Jupiter-like planets: An analytical solution and its numerical validation

    Science.gov (United States)

    Kong, Dali; Zhang, Keke; Schubert, Gerald

    2017-02-01

    It is expected that the Juno spacecraft will provide an accurate spectrum of the Jovian zonal gravitational coefficients that would be affected by both the deep zonal flow, if it exists, and the basic rotational distortion. We derive the first analytical solution, under the spheroidal-shape approximation, for the density anomaly induced by an internal zonal flow in rapidly rotating Jupiter-like planets. We compare the density anomaly of the analytical solution to that obtained from a fully numerical solution based on a three-dimensional finite element method; the two show excellent agreement. We apply the analytical solution to a rapidly rotating Jupiter-like planet and show that there exists a close relationship between the spatial structure of the zonal flow and the spectrum of zonal gravitational coefficients. We check the accuracy of the spheroidal-shape approximation by computing both the spheroidal and non-spheroidal solutions with exactly the same physical parameters. We also discuss implications of the new analytical solution for interpreting the future high-precision gravitational measurements of the Juno spacecraft.

  3. Validation of SPME-GCMS method for the analysis of virgin olive oil volatiles responsible for sensory defects.

    Science.gov (United States)

    Romero, I; García-González, D L; Aparicio-Ruiz, R; Morales, M T

    2015-03-01

    Volatile compounds are responsible for the aroma of virgin olive oil and also for its quality. The high number and different nature of volatile compounds drive to the need of a reliable analytical method that allows their proper quantification to explain the standard method of panel test. Although there are some analytical solutions available, they have not been validated and the regulatory bodies are reluctant to adopt them since they can be subjected to unknown errors. In this regards, the European Union has encouraged the validation of these analytical tools through the research program Horizon2020, which involves gaining knowledge from the analytical properties of the chemical methods for sensory assessment. This work is focused on the analytical validation of the methodology used to determine the actual concentration of volatiles in virgin olive oils when applying SPME-GCMS. The validation process includes the calibration curves for 29 volatile compounds responsible for the most common sensory perceptions in virgin olive oils, the determination of their working ranges with linear response, the detection and quantification limits, the sensitivity, the accuracy estimated as trueness and precision and the selectivity. Sixty-seven percent of the compounds presented a relative standard deviation in repeatability lower than 10%, and this percentage rises to 95% in lampante virgin olive oils. The accuracy was established in 97% of the studied volatile compounds. Finally, an empirical example of the ability of the method to discriminate virgin olive oils of different categories (extra virgin, virgin, ordinary and lampante) by the quantification of their volatiles is provided.

  4. Gas Chromatography Method of Cleaning Validation Process for 2-Propanol Residue Determination in Pharmaceutical Manufacturing Equipment

    Directory of Open Access Journals (Sweden)

    Łukasz Czubak

    2014-07-01

    Full Text Available Cleaning validation is an integral operation of good manufacturing practice in pharmaceutical industry. The aim of this study was to validate simple analytical method for detection of 2-propanol residue in equipment, which is likely contaminated with 2-propanol, usually used in the production area. The gas chromatography with flame ionization detection (GC-FID method was validated on a GC system using DB-FFAP capillary column at the flow rate of 4.9 mL/min. The calibration curve was linear over concentration range from 2.8µg/mL to 110.7µg/mL with a correlation coefficient equal to 0.99981. The detection limit (LOD and quantitation limit (LOQ were 1.1µg/mL and 2.8µg/mL, respectively. The simplicity of gas chromatography method makes it useful for routine analysis of 2-propanol residue and is an alternative to corresponding methods.

  5. Approximate Analytic Solutions for the Two-Phase Stefan Problem Using the Adomian Decomposition Method

    Directory of Open Access Journals (Sweden)

    Xiao-Ying Qin

    2014-01-01

    Full Text Available An Adomian decomposition method (ADM is applied to solve a two-phase Stefan problem that describes the pure metal solidification process. In contrast to traditional analytical methods, ADM avoids complex mathematical derivations and does not require coordinate transformation for elimination of the unknown moving boundary. Based on polynomial approximations for some known and unknown boundary functions, approximate analytic solutions for the model with undetermined coefficients are obtained using ADM. Substitution of these expressions into other equations and boundary conditions of the model generates some function identities with the undetermined coefficients. By determining these coefficients, approximate analytic solutions for the model are obtained. A concrete example of the solution shows that this method can easily be implemented in MATLAB and has a fast convergence rate. This is an efficient method for finding approximate analytic solutions for the Stefan and the inverse Stefan problems.

  6. Matrix Analytic Methods in Applied Probability with a View towards Engineering Applications

    DEFF Research Database (Denmark)

    Nielsen, Bo Friis

    is an essential building block within matrix analytic methods in queueing theory pioneered by Neuts and coauthors. The theory of matrix analytic methods is appealing from a practical point of view as many systems can be analytically and numerically evaluated using this approach. In this thesis we present...... contributions to the theoretical development of the field of matrix analytic methods including an extension to a multivariate setting. We further demonstrate the applicability of the theory, giving examples from telecommunications engineering and computer science. The thesis is based on a number of original...... is devoted to discussion of parameter estimation in the models described in Chapter 2. We give a very brief review of current estimation methods while focusing on our own contributions. Chapters 4 and 5 contain different aspects of applications. The MAP is a versatile tool in sensitivity analyses...

  7. Approximation analytical solutions for a unified plasma sheath model by double decomposition method

    Institute of Scientific and Technical Information of China (English)

    FangJin-Qing

    1998-01-01

    A unified plasma sheath model and its potential equation are proposed.Any higher-order approximation analytical solutions for the unified plasma sheath potential equation are derived by double decomposition method.

  8. Diclofenac quantification: analytical attributes of a spectrophotometric method

    OpenAIRE

    Monzón, Celina M.; Sarno, María del C.; Delfino, Mario R. (h)

    2011-01-01

    An spectrophotometric UV-visible technique used to quantify diclofenac and its application to pharmaceutical preparations is described, based on diclofenac oxidation by Fe(III) in the presence of ophenanthroline. The formation of tris (o-phenanthroline)-Fe(II) complex (ferroin) upon diclofenac reaction was investigated. Absorbance of ferroin complex was measured at 506 nm. This method was tested on 50 mg tablets. Operating with placebos, it was found that excipients do not interfere with the ...

  9. Advanced and In Situ Analytical Methods for Solar Fuel Materials.

    Science.gov (United States)

    Chan, Candace K; Tüysüz, Harun; Braun, Artur; Ranjan, Chinmoy; La Mantia, Fabio; Miller, Benjamin K; Zhang, Liuxian; Crozier, Peter A; Haber, Joel A; Gregoire, John M; Park, Hyun S; Batchellor, Adam S; Trotochaud, Lena; Boettcher, Shannon W

    2016-01-01

    In situ and operando techniques can play important roles in the development of better performing photoelectrodes, photocatalysts, and electrocatalysts by helping to elucidate crucial intermediates and mechanistic steps. The development of high throughput screening methods has also accelerated the evaluation of relevant photoelectrochemical and electrochemical properties for new solar fuel materials. In this chapter, several in situ and high throughput characterization tools are discussed in detail along with their impact on our understanding of solar fuel materials.

  10. A method of calculating the Jost function for analytic potentials

    Energy Technology Data Exchange (ETDEWEB)

    Rakityansky, S.A. [University of South Africa (UNISA), Pretoria (South Africa). Dept. of Physics; Sofianos, S.A. [Joint Inst. for Nuclear Research, Dubna (Russian Federation); Amos, K. [Melbourne Univ., Parkville, VIC (Australia). School of Physics

    1995-05-10

    A combination of the variable-constant and complex coordinate rotation methods is used to solve the two-body Schroedinger equation. The equation is replaced by a system of linear first-order differential equations, which enables one to perform direct calculation of the Jost function for all complex momenta of physical interest including the spectral points corresponding to bound and resonance states. 16 refs., 2 tabs., 2 figs.

  11. Analytical methods applied to diverse types of Brazilian propolis

    Science.gov (United States)

    2011-01-01

    Propolis is a bee product, composed mainly of plant resins and beeswax, therefore its chemical composition varies due to the geographic and plant origins of these resins, as well as the species of bee. Brazil is an important supplier of propolis on the world market and, although green colored propolis from the southeast is the most known and studied, several other types of propolis from Apis mellifera and native stingless bees (also called cerumen) can be found. Propolis is usually consumed as an extract, so the type of solvent and extractive procedures employed further affect its composition. Methods used for the extraction; analysis the percentage of resins, wax and insoluble material in crude propolis; determination of phenolic, flavonoid, amino acid and heavy metal contents are reviewed herein. Different chromatographic methods applied to the separation, identification and quantification of Brazilian propolis components and their relative strengths are discussed; as well as direct insertion mass spectrometry fingerprinting. Propolis has been used as a popular remedy for several centuries for a wide array of ailments. Its antimicrobial properties, present in propolis from different origins, have been extensively studied. But, more recently, anti-parasitic, anti-viral/immune stimulating, healing, anti-tumor, anti-inflammatory, antioxidant and analgesic activities of diverse types of Brazilian propolis have been evaluated. The most common methods employed and overviews of their relative results are presented. PMID:21631940

  12. Analytical methods applied to diverse types of Brazilian propolis

    Directory of Open Access Journals (Sweden)

    Marcucci Maria

    2011-06-01

    Full Text Available Abstract Propolis is a bee product, composed mainly of plant resins and beeswax, therefore its chemical composition varies due to the geographic and plant origins of these resins, as well as the species of bee. Brazil is an important supplier of propolis on the world market and, although green colored propolis from the southeast is the most known and studied, several other types of propolis from Apis mellifera and native stingless bees (also called cerumen can be found. Propolis is usually consumed as an extract, so the type of solvent and extractive procedures employed further affect its composition. Methods used for the extraction; analysis the percentage of resins, wax and insoluble material in crude propolis; determination of phenolic, flavonoid, amino acid and heavy metal contents are reviewed herein. Different chromatographic methods applied to the separation, identification and quantification of Brazilian propolis components and their relative strengths are discussed; as well as direct insertion mass spectrometry fingerprinting. Propolis has been used as a popular remedy for several centuries for a wide array of ailments. Its antimicrobial properties, present in propolis from different origins, have been extensively studied. But, more recently, anti-parasitic, anti-viral/immune stimulating, healing, anti-tumor, anti-inflammatory, antioxidant and analgesic activities of diverse types of Brazilian propolis have been evaluated. The most common methods employed and overviews of their relative results are presented.

  13. Assessment of Two Analytical Methods in Solving the Linear and Nonlinear Elastic Beam Deformation Problems

    DEFF Research Database (Denmark)

    Barari, Amin; Ganjavi, B.; Jeloudar, M. Ghanbari

    2010-01-01

    Purpose – In the last two decades with the rapid development of nonlinear science, there has appeared ever-increasing interest of scientists and engineers in the analytical techniques for nonlinear problems. This paper considers linear and nonlinear systems that are not only regarded as general...... and fluid mechanics. Design/methodology/approach – Two new but powerful analytical methods, namely, He's VIM and HPM, are introduced to solve some boundary value problems in structural engineering and fluid mechanics. Findings – Analytical solutions often fit under classical perturbation methods. However...

  14. Analytical performance of two miniaturised extraction methods for triclosan and methyltriclosan, in fish roe and surimi samples.

    Science.gov (United States)

    Gonzalo-Lumbreras, R; Sanz-Landaluze, J; Cámara, C

    2014-03-01

    A new and reliable miniaturised QuEChERS-based extraction method combined with a dispersive SPE cleanup procedure for extracting triclosan and methyltriclosan from fish roe and surimi samples was proposed. The effectiveness of different extraction/partition conditions for QuEChERS method was systematically investigated, and the use of acetonitrile extraction solvent and MgSO4, PSA, C18 and Florisil as cleanup reagents was recommended in the final method. Other method based on ultrasonic extraction with ethylacetate and clean-up with SPE was also evaluated for these samples. Different polymeric and silica sorbents for clean up were tested and the combination of Florisil and PSA was finally selected. The performance of these miniaturised sample preparation methods combined with GC-MS with quadrupole detection were compared. Extraction efficiency as well as cleaning effectiveness, laboriousness and speed were taken as criteria for method evaluation. Satisfactory validation parameters, such as linearity, recovery, precision and LODs and LOQs for both developed analytical methods were obtained from fish roe and surimi samples. Finally, both methods were applied to real samples. The sensitivity of the proposed methods was good enough to ensure reliable determination of target analytes at concentration levels commonly found in this kind of samples.

  15. An analytical investigation on unsteady motion of vertically falling spherical particles in non-Newtonian fluid by Collocation Method

    Directory of Open Access Journals (Sweden)

    M. Rahimi-Gorji

    2015-06-01

    Full Text Available An analytical investigation is applied for unsteady motion of a rigid spherical particle in a quiescent shear-thinning power-law fluid. The results were compared with those obtained from Collocation Method (CM and the established Numerical Method (Fourth order Runge–Kutta scheme. It was shown that CM gave accurate results. Collocation Method (CM and Numerical Method are used to solve the present problem. We obtained that the CM which was used to solve such nonlinear differential equation with fractional power is simpler and more accurate than series method such as HPM which was used in some previous works by others but the new method named Akbari-Ganji’s Method (AGM is an accurate and simple method which is slower than CM for solving such problems. The terminal settling velocity—that is the velocity at which the net forces on a falling particle eliminate—for three different spherical particles (made of plastic, glass and steel and three flow behavior index n, in three sets of power-law non-Newtonian fluids was investigated, based on polynomial solution (CM. Analytical results obtained indicated that the time of reaching the terminal velocity in a falling procedure is significantly increased with growing of the particle size that validated with Numerical Method. Further, with approaching flow behavior to Newtonian behavior from shear-thinning properties of flow (n → 1, the transient time to achieving the terminal settling velocity is decreased.

  16. SEMI-ANALYTICAL FINITE ELEMENT METHOD FOR FICTITIOUS CRACK MODEL IN FRACTURE MECHANICS OF CONCRETE

    Institute of Scientific and Technical Information of China (English)

    王承强; 郑长良

    2004-01-01

    Based on the Hamiltonian governing equations of plane elasticity for sectorial domain, the variable separation and eigenfunction expansion techniques were employed to develop a novel analytical finite element for the fictitious crack model in fracture mechanics of concrete. The new analytical element can be implemented into FEM program systems to solve fictitious crack propagation problems for concrete cracked plates with arbitrary shapes and loads. Numerical results indicate that the method is more efficient and accurate than ordinary finite element method.

  17. Homogenous Balance Method and Exact Analytical Solutions for Whitham-Broer-Kaup Equations in Shallow Water

    Institute of Scientific and Technical Information of China (English)

    XIAZhi

    2004-01-01

    Based on the homogenous balance method and with the help of mathematica, the Backlund transformation and the transfer heat equation are derived. Analyzing the heat-transfer equation, the multiple soliton solutions and other exact analytical solution for Whitham-Broer-Kaup equations(WBK) are derived. These solutions contain Fan's, Xie's and Yan's results and other new types of analytical solutions, such as rational function solutions and periodic solutions. The method can also be applied to solve more nonlinear differential equations.

  18. Analytical Methods for Environmental Risk Assessment of Acid Sulfate Soils: A Review

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Assessment of acid sulfate soil risk is an important step for acid sulfate soil management and its reliability depends very much on the suitability and accuracy of various analytical methods for estimating sulfide-derived potential acidity, actual acidity and acid-neutralizing capacity in acid sulfate soils. This paper critically reviews various analytical methods that are currently used for determination of the above parameters, as well as their implications for environmental risk assessment of acid sulfate soils.

  19. An Approximate Analytical Method for the Evaluation of the Concentrations and Current for Hybrid Enzyme Biosensor

    OpenAIRE

    2013-01-01

    Mathematical modeling of amperometric biosensor with cyclic reaction is discussed. Analytical expressions pertaining to the concentration of substrate, cosubstrate, reducing agent and medial product and current for hybrid enzyme biosensor are obtained in terms of Thiele module and saturation parameters. In this paper, a powerful analytical method, called homotopy analysis method (HAM) is used to solve the system of nonlinear differential equations. Furthermore, in this work the numerical simu...

  20. Analytical validation considerations of multiplex mass-spectrometry-based proteomic platforms for measuring protein biomarkers.

    Science.gov (United States)

    Boja, Emily S; Fehniger, Thomas E; Baker, Mark S; Marko-Varga, György; Rodriguez, Henry

    2014-12-01

    Protein biomarker discovery and validation in current omics era are vital for healthcare professionals to improve diagnosis, detect cancers at an early stage, identify the likelihood of cancer recurrence, stratify stages with differential survival outcomes, and monitor therapeutic responses. The success of such biomarkers would have a huge impact on how we improve the diagnosis and treatment of patients and alleviate the financial burden of healthcare systems. In the past, the genomics community (mostly through large-scale, deep genomic sequencing technologies) has been steadily improving our understanding of the molecular basis of disease, with a number of biomarker panels already authorized by the U.S. Food and Drug Administration (FDA) for clinical use (e.g., MammaPrint, two recently cleared devices using next-generation sequencing platforms to detect DNA changes in the cystic fibrosis transmembrane conductance regulator (CFTR) gene). Clinical proteomics, on the other hand, albeit its ability to delineate the functional units of a cell, more likely driving the phenotypic differences of a disease (i.e., proteins and protein-protein interaction networks and signaling pathways underlying the disease), "staggers" to make a significant impact with only an average ∼ 1.5 protein biomarkers per year approved by the FDA over the past 15-20 years. This statistic itself raises the concern that major roadblocks have been impeding an efficient transition of protein marker candidates in biomarker development despite major technological advances in proteomics in recent years.

  1. Validity of Particle-Counting Method Using Laser-Light Scattering for Detecting Platelet Aggregation in Diabetic Patients

    Science.gov (United States)

    Nakadate, Hiromichi; Sekizuka, Eiichi; Minamitani, Haruyuki

    We aimed to study the validity of a new analytical approach that reflected the phase from platelet activation to the formation of small platelet aggregates. We hoped that this new approach would enable us to use the particle-counting method with laser-light scattering to measure platelet aggregation in healthy controls and in diabetic patients without complications. We measured agonist-induced platelet aggregation for 10 min. Agonist was added to the platelet-rich plasma 1 min after measurement started. We compared the total scattered light intensity from small aggregates over a 10-min period (established analytical approach) and that over a 2-min period from 1 to 3 min after measurement started (new analytical approach). Consequently platelet aggregation in diabetics with HbA1c ≥ 6.5% was significantly greater than in healthy controls by both analytical approaches. However, platelet aggregation in diabetics with HbA1c < 6.5%, i.e. patients in the early stages of diabetes, was significantly greater than in healthy controls only by the new analytical approach, not by the established analytical approach. These results suggest that platelet aggregation as detected by the particle-counting method using laser-light scattering could be applied in clinical examinations by our new analytical approach.

  2. A Vocal-Based Analytical Method for Goose Behaviour Recognition

    Directory of Open Access Journals (Sweden)

    Henrik Karstoft

    2012-03-01

    Full Text Available Since human-wildlife conflicts are increasing, the development of cost-effective methods for reducing damage or conflict levels is important in wildlife management. A wide range of devices to detect and deter animals causing conflict are used for this purpose, although their effectiveness is often highly variable, due to habituation to disruptive or disturbing stimuli. Automated recognition of behaviours could form a critical component of a system capable of altering the disruptive stimuli to avoid this. In this paper we present a novel method to automatically recognise goose behaviour based on vocalisations from flocks of free-living barnacle geese (Branta leucopsis. The geese were observed and recorded in a natural environment, using a shielded shotgun microphone. The classification used Support Vector Machines (SVMs, which had been trained with labeled data. Greenwood Function Cepstral Coefficients (GFCC were used as features for the pattern recognition algorithm, as they can be adjusted to the hearing capabilities of different species. Three behaviours are classified based in this approach, and the method achieves a good recognition of foraging behaviour (86–97% sensitivity, 89–98% precision and a reasonable recognition of flushing (79–86%, 66–80% and landing behaviour(73–91%, 79–92%. The Support Vector Machine has proven to be a robust classifier for this kind of classification, as generality and non-linearcapabilities are important. We conclude that vocalisations can be used to automatically detect behaviour of conflict wildlife species, and as such, may be used as an integrated part of awildlife management system.

  3. An Efficient Certificate Status Validation Method for Mobile Communication

    Institute of Scientific and Technical Information of China (English)

    ZHOUYongbin; QINGSihan; ZHANGZhenfeng; JIQingguang

    2004-01-01

    The huge success of mobile telephone and such other wireless digital devices have transformed business and the Inter'net. In order to protect the security of mobile commerce transaction, WAP forum specified the WAP security protocol and defined WPKI architecture. Certificate status checking is one of the challenging issues of PKI in wired settings~ and it is more challenging in the wireless world (that is WPKI here) due to the limitations of mobile devices. In this paper, several mechanisms for certificate status validation are summarized and compared, and a new efficient certificate status validation method for WPKI is presented based on commutative hashing and a variation of dynamic Merkle hash tree. The newly proposed scheme has the advantages of being efficient and secure. The computation of the tree is independent of the nodes’ relative location in the hash tree, thus simplifying the computation and verification process. The proposed scheme is compatible with both X.509 certificate and WTLS certificate.

  4. Development and validation of a high performance liquid chromatography method for oligodeoxynucleotides determination in a novel coagel-based formulation

    Directory of Open Access Journals (Sweden)

    Gabriela V. Ullio-Gamboa

    2015-06-01

    However, due to inter-assay variability and accuracy problems associated with the afore mentioned methods, we have developed and validated an isocratic high performance liquid chromatographic (HPLC for analytical determination of PS-ODN containing unmethylated CpG motifs (CpG-ODN. Validation under Food and Drug Administration (FDA guidelines of the analytical parameters include: linearity (r2 0.9996, LOD (0.86 μg/ml and LOQ (6.25 μg/ml, intra (0.19–3.37% and inter-day precision (0.63–3.75% expressed as relative standard deviation (RSD, and robustness parameters (less than 2.80%. Using this method, recoveries ranging from 89.9% to 99.9% were obtained. Thus, this method provides a simple, sensitive, precise and reproducible examination which can be readily adapted for the assessment of CpG-ODN in different pharmaceutical preparations.

  5. A two-dimensional analytical model and experimental validation of garter stitch knitted shape memory alloy actuator architecture

    Science.gov (United States)

    Abel, Julianna; Luntz, Jonathan; Brei, Diann

    2012-08-01

    Active knits are a unique architectural approach to meeting emerging smart structure needs for distributed high strain actuation with simultaneous force generation. This paper presents an analytical state-based model for predicting the actuation response of a shape memory alloy (SMA) garter knit textile. Garter knits generate significant contraction against moderate to large loads when heated, due to the continuous interlocked network of loops of SMA wire. For this knit architecture, the states of operation are defined on the basis of the thermal and mechanical loading of the textile, the resulting phase change of the SMA, and the load path followed to that state. Transitions between these operational states induce either stick or slip frictional forces depending upon the state and path, which affect the actuation response. A load-extension model of the textile is derived for each operational state using elastica theory and Euler-Bernoulli beam bending for the large deformations within a loop of wire based on the stress-strain behavior of the SMA material. This provides kinematic and kinetic relations which scale to form analytical transcendental expressions for the net actuation motion against an external load. This model was validated experimentally for an SMA garter knit textile over a range of applied forces with good correlation for both the load-extension behavior in each state as well as the net motion produced during the actuation cycle (250% recoverable strain and over 50% actuation). The two-dimensional analytical model of the garter stitch active knit provides the ability to predict the kinetic actuation performance, providing the basis for the design and synthesis of large stroke, large force distributed actuators that employ this novel architecture.

  6. Development and validation of methods for the trace determination of phthalates in sludge and vegetables.

    Science.gov (United States)

    Sablayrolles, Caroline; Montréjaud-Vignoles, Mireille; Benanou, David; Patria, Lucie; Treilhou, Michel

    2005-04-29

    A routine method which is simple, quick and precise has been set up and validated for phthalate analysis in environmental samples (tomato plants and sewage sludges). Six phthalates have been studied simultaneously: dimethylphthalate, diethylphthalate, di-n-butylphthalate, n-butylbenzylphthalate, di-2-ethyl-hexyl phthalate (DEHP) and di-n-octylphthalate. Optimization of sample, solvent extraction uses a Soxtec apparatus and extract purification with an a solid-phase extraction cartridge allows between 90 and 110% recovery of phthalates. Precise, sensitive and selective identification and quantifying of analytes is by GC-MS in the single ion monitoring mode. This protocol allows analytes with concentrations as low as 10 microg/kg dry matter (DM) to be determined from small (1-2 g DM) samples. This analytical method has been applied to the phthalate transfer study for agricultural recycling of sludges, where phthalate bioavailability has been studied in aquiculture using two types of experiments. Tomatoes have been grown in containers where the trace organics have been directly introduced as pure substances, and in a second experiment under the same growth conditions, sewage sludge has replaced the pure substances. Transfer of these trace organics has been followed into the various parts of the tomato plant and in general only the DEHP is worthy of note although its percentage transfer remains very low even in an experiment designed to maximize this.

  7. Analytical solution of advection–diffusion equation in heterogeneous infinite medium using Green’s function method

    Indian Academy of Sciences (India)

    Abhishek Sanskrityayn; Naveen Kumar

    2016-12-01

    Some analytical solutions of one-dimensional advection–diffusion equation (ADE) with variable dispersion coefficient and velocity are obtained using Green’s function method (GFM). The variability attributes to the heterogeneity of hydro-geological media like river bed or aquifer in more general ways than that in the previous works. Dispersion coefficient is considered temporally dependent, while velocity is considered spatially and temporally dependent. The spatial dependence is considered to be linear and temporal dependence is considered to be of linear, exponential and asymptotic. The spatio-temporal dependence of velocity is considered in three ways. Results of previous works are also derived validating the results of the present work. To use GFM, a moving coordinate transformation is developed through which this ADE is reduced into a form, whose analytical solution is already known. Analytical solutions are obtained for the pollutant’s mass dispersion from an instantaneous point source as well as from a continuous point source in a heterogeneous medium. The effect of such dependence on the mass transport is explained through the illustrations of the analytical solutions.

  8. Analytical Chemistry Laboratory (ACL) procedure compendium. Volume 4, Organic methods

    Energy Technology Data Exchange (ETDEWEB)

    1993-08-01

    This interim notice covers the following: extractable organic halides in solids, total organic halides, analysis by gas chromatography/Fourier transform-infrared spectroscopy, hexadecane extracts for volatile organic compounds, GC/MS analysis of VOCs, GC/MS analysis of methanol extracts of cryogenic vapor samples, screening of semivolatile organic extracts, GPC cleanup for semivolatiles, sample preparation for GC/MS for semi-VOCs, analysis for pesticides/PCBs by GC with electron capture detection, sample preparation for pesticides/PCBs in water and soil sediment, report preparation, Florisil column cleanup for pesticide/PCBs, silica gel and acid-base partition cleanup of samples for semi-VOCs, concentrate acid wash cleanup, carbon determination in solids using Coulometrics` CO{sub 2} coulometer, determination of total carbon/total organic carbon/total inorganic carbon in radioactive liquids/soils/sludges by hot persulfate method, analysis of solids for carbonates using Coulometrics` Model 5011 coulometer, and soxhlet extraction.

  9. Validação de método analítico espectrofotométrico UV para determinação de ácido úsnico em lipossomas Validation of a UV-spectrophotometric analytical method for the determination of usnic acid in liposomes

    Directory of Open Access Journals (Sweden)

    Marigilson Pontes de Siqueira-Moura

    2008-12-01

    Full Text Available O ácido úsnico (AU é um composto de origem liquênica e tem demonstrado importantes atividades biológicas, tais como: antitumoral, antimicrobiano, antiviral, antiproliferativo e antiinflamatório. Os lipossomas são vesículas lipídicas contendo espaço aquoso interno e têm sido utilizados como carreadores coloidais de fármacos, principalmente na terapêutica de câncer e infecções bacterianas e fúngicas. O objetivo desse trabalho foi desenvolver e validar um método espectrofotométrico UV para determinação de ácido úsnico em lipossomas. Os parâmetros de validação linearidade, precisão, exatidão, robustez, limites de detecção e quantificação foram determinados segundo diretrizes internacionais de padronização e Farmacopéia Americana. A faixa de linearidade foi de 3 a 15 µg.mL-1, a equação de regressão: absorbância = 0,070 x [AU] (µg.mL-1 + 0,013 e r = 0,9997. A repetibilidade (coeficiente de variação do método foi 1,96% e a precisão intermediária indicou que a diferença entre as médias foi estatisticamente insignificante (P The secondary lichen metabolite usnic acid [2,6-diacetyl-7,9-dihydroxy-8,9b-dimethyl-1,3(2H,9bH-dibenzofuran] has demonstrated pharmacological potential activities such as antitumor, antimicrobial, antiviral, antiproliferative, and anti-inflammatory. Liposomes are vesicles composed of phospholipid bilayers surrounding aqueous compartments and they have been used as colloidal drug carriers. The aim of this study was to develop and validate a quantitative UV spectrophotometric method for determination of usnic acid in liposomal formulations. The validation parameters were assessed according to The International Conference on Harmonization (ICH and American Pharmacopoeia guidelines. The linearity range was of 3-15 µg.mL-1, regression equation: absorbance = 0.070 x UA concentration (µg.mL-1 + 0.013, and r = 0.9997. The repeatability (relative standard deviation of the method was 1.96% and

  10. Development and validation of simple RP-HPLC-PDA analytical protocol for zileuton assisted with Design of Experiments for robustness determination

    Directory of Open Access Journals (Sweden)

    Saurabh B. Ganorkar

    2017-02-01

    Full Text Available A simple, rapid, sensitive, robust, stability-indicating RP-HPLC-PDA analytical protocol was developed and validated for the analysis of zileuton racemate in bulk and in tablet formulation. Development of method and resolution of degradation products from forced; hydrolytic (acidic, basic, neutral, oxidative, photolytic (acidic, basic, neutral, solid state and thermal (dry heat degradation was achieved on a LC – GC Qualisil BDS C18 column (250 mm × 4.6 mm × 5 μm by isocratic mode at ambient temperature, employing a mobile phase methanol and (0.2%, v/v orthophosphoric acid in ratio of (80:20, v/v at a flow rate of 1.0 mL min−1 and detection at 260 nm. ‘Design of Experiments’ (DOE employing ‘Central Composite Design’ (CCD and ‘Response Surface Methodology’ (RSM were applied as an advancement to traditional ‘One Variable at Time’ (OVAT approach to evaluate the effects of variations in selected factors (methanol content, flow rate, concentration of orthophosphoric acid as graphical interpretation for robustness and statistical interpretation was achieved with Multiple Linear Regression (MLR and ANOVA. The method succeeded over the validation parameters: linearity, precision, accuracy, limit of detection and limit of quantitation, and robustness. The method was applied effectively for analysis of in-house zileuton tablets.

  11. An analytical method of estimating Value-at-Risk on the Belgrade Stock Exchange

    Directory of Open Access Journals (Sweden)

    Obadović Milica D.

    2009-01-01

    Full Text Available This paper presents market risk evaluation for a portfolio consisting of shares that are continuously traded on the Belgrade Stock Exchange, by applying the Value-at-Risk model - the analytical method. It describes the manner of analytical method application and compares the results obtained by implementing this method at different confidence levels. Method verification was carried out on the basis of the failure rate that demonstrated the confidence level for which this method was acceptable in view of the given conditions.

  12. A novel method for analytically solving a radial advection-dispersion equation

    Science.gov (United States)

    Lai, Keng-Hsin; Liu, Chen-Wuing; Liang, Ching-Ping; Chen, Jui-Sheng; Sie, Bing-Ruei

    2016-11-01

    An analytical solution for solute transport in a radial flow field has a variety of practical applications in the study of the transport in push-pull/divergent/convergent flow tracer tests, aquifer remediation by pumping and aquifer storage and recovery. However, an analytical solution for radial advective-dispersive transport has been proven very difficult to develop and relatively few in subsurface hydrology have made efforts to do so, because variable coefficients in the governing partial differential equations. Most of the solutions for radial advective-dispersive transport presented in the literature have generally been solved semi-analytically with the final concentration values being obtained with the help of a numerical Laplace inversion. This study presents a novel solution strategy for analytically solving the radial advective-dispersive transport problem. A Laplace transform with respect to the time variable and a generalized integral transform technique with respect to the spatial variable are first performed to convert the transient governing partial differential equations into an algebraic equation. Subsequently, the algebraic equation is solved using simple algebraic manipulations, easily yielding the solution in the transformed domain. The solution in the original domain is ultimately obtained by successive applications of the Laplace and corresponding generalized integral transform inversions. A convergent flow tracer test is used to demonstrate the robustness of the proposed method for deriving an exact analytical solution to the radial advective-dispersive transport problem. The developed analytical solution is verified against a semi-analytical solution taken from the literature. The results show perfect agreement between our exact analytical solution and the semi-analytical solution. The solution method presented in this study can be applied to create more comprehensive analytical models for a great variety of radial advective

  13. Analytical recovery of protozoan enumeration methods: have drinking water QMRA models corrected or created bias?

    Science.gov (United States)

    Schmidt, P J; Emelko, M B; Thompson, M E

    2013-05-01

    Quantitative microbial risk assessment (QMRA) is a tool to evaluate the potential implications of pathogens in a water supply or other media and is of increasing interest to regulators. In the case of potentially pathogenic protozoa (e.g. Cryptosporidium oocysts and Giardia cysts), it is well known that the methods used to enumerate (oo)cysts in samples of water and other media can have low and highly variable analytical recovery. In these applications, QMRA has evolved from ignoring analytical recovery to addressing it in point-estimates of risk, and then to addressing variation of analytical recovery in Monte Carlo risk assessments. Often, variation of analytical recovery is addressed in exposure assessment by dividing concentration values that were obtained without consideration of analytical recovery by random beta-distributed recovery values. A simple mathematical proof is provided to demonstrate that this conventional approach to address non-constant analytical recovery in drinking water QMRA will lead to overestimation of mean pathogen concentrations. The bias, which can exceed an order of magnitude, is greatest when low analytical recovery values are common. A simulated dataset is analyzed using a diverse set of approaches to obtain distributions representing temporal variation in the oocyst concentration, and mean annual risk is then computed from each concentration distribution using a simple risk model. This illustrative example demonstrates that the bias associated with mishandling non-constant analytical recovery and non-detect samples can cause drinking water systems to be erroneously classified as surpassing risk thresholds.

  14. An Other Perspective on Personality: Meta-Analytic Integration of Observers' Accuracy and Predictive Validity

    Science.gov (United States)

    Connelly, Brian S.; Ones, Deniz S.

    2010-01-01

    The bulk of personality research has been built from self-report measures of personality. However, collecting personality ratings from other-raters, such as family, friends, and even strangers, is a dramatically underutilized method that allows better explanation and prediction of personality's role in many domains of psychology. Drawing…

  15. An introduction to clinical microeconomic analysis: purposes and analytic methods.

    Science.gov (United States)

    Weintraub, W S; Mauldin, P D; Becker, E R

    1994-06-01

    The recent concern with health care economics has fostered the development of a new discipline that is generally called clinical microeconomics. This is a discipline in which microeconomic methods are used to study the economics of specific medical therapies. It is possible to perform stand alone cost analyses, but more profound insight into the medical decision making process may be accomplished by combining cost studies with measures of outcome. This is most often accomplished with cost-effectiveness or cost-utility studies. In cost-effectiveness studies there is one measure of outcome, often death. In cost-utility studies there are multiple measures of outcome, which must be grouped together to give an overall picture of outcome or utility. There are theoretical limitations to the determination of utility that must be accepted to perform this type of analysis. A summary statement of outcome is quality adjusted life years (QALYs), which is utility time socially discounted survival. Discounting is used because people value a year of future life less than a year of present life. Costs are made up of in-hospital direct, professional, follow-up direct, and follow-up indirect costs. Direct costs are for medical services. Indirect costs reflect opportunity costs such as lost time at work. Cost estimates are often based on marginal costs, or the cost for one additional procedure of the same type. Finally an overall statistic may be generated as cost per unit increase in effectiveness, such as dollars per QALY.(ABSTRACT TRUNCATED AT 250 WORDS)

  16. Development of an Analytical System for Determination of Free Acid via a Joint Method Combining Density and Conductivity Measurement

    Institute of Scientific and Technical Information of China (English)

    2011-01-01

    Determination of free acid plays an important role in spent nuclear fuel reprocessing. It is necessary to develop a rapid analytical device and method for measuring free acid. A novel analytical system and method was studied to monitor the acidity

  17. Determination of formaldehyde in food and feed by an in-house validated HPLC method.

    Science.gov (United States)

    Wahed, P; Razzaq, Md A; Dharmapuri, S; Corrales, M

    2016-07-01

    Formalin is carcinogenic and is detrimental to public health. The illegal addition of formalin (37% formaldehyde and 14% methanol) to foods to extend their shelf-life is considered to be a common practice in Bangladesh. The lack of accurate methods and the ubiquitous presence of formaldehyde in foods make the detection of illegally added formalin challenging. With the aim of helping regulatory authorities, a sensitive high performance liquid chromatography method was validated for the quantitative determination of formaldehyde in mango, fish and milk. The method was fit-for-purpose and showed good analytical performance in terms of specificity, linearity, precision, recovery and robustness. The expanded uncertainty was <35%. The validated method was applied to screen samples of fruits, vegetables, fresh fish, milk and fish feed collected from different local markets in Dhaka, Bangladesh. Levels of formaldehyde in food samples were compared with published data. The applicability of the method in different food matrices might mean it has potential as a reference standard method.

  18. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina para espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method's performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 +- 11,70)mug.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10{mu}g.L{sup -1}. The

  19. Validation of a hybrid life-cycle inventory analysis method.

    Science.gov (United States)

    Crawford, Robert H

    2008-08-01

    The life-cycle inventory analysis step of a life-cycle assessment (LCA) may currently suffer from several limitations, mainly concerned with the use of incomplete and unreliable data sources and methods of assessment. Many past LCA studies have used traditional inventory analysis methods, namely process analysis and input-output analysis. More recently, hybrid inventory analysis methods have been developed, combining these two traditional methods in an attempt to minimise their limitations. In light of recent improvements, these hybrid methods need to be compared and validated, as these too have been considered to have several limitations. This paper evaluates a recently developed hybrid inventory analysis method which aims to improve the limitations of previous methods. It was found that the truncation associated with process analysis can be up to 87%, reflecting the considerable shortcomings in the quantity of process data currently available. Capital inputs were found to account for up to 22% of the total inputs to a particular product. These findings suggest that current best-practice methods are sufficiently accurate for most typical applications, but this is heavily dependent upon data quality and availability. The use of input-output data assists in improving the system boundary completeness of life-cycle inventories. However, the use of input-output analysis alone does not always provide an accurate model for replacing process data. Further improvements in the quantity of process data currently available are needed to increase the reliability of life-cycle inventories.

  20. Meteorological radar methods for validating space observations of precipitation

    Science.gov (United States)

    Thiele, Otto W.

    1991-01-01

    Meteorological approaches to verification of space measurements of rainfall are examined; validation of Tropical Rainfall Measuring Mission (TRMM) observations is expected to depend significantly on ground-based radars. Two methods of comparison are initially contemplated. TRMM rainfall data over time periods of a month for large areas (500 x 500 km) are averaged and compared with similarly averaged ground truth measurements. Both the rainfall and height distribution data from TRMM are compared with the instantaneous values observed at one or more 'ground truth' stations and from airborne radar and radiometers as available.

  1. Approximate Analytical Solutions of the Regularized Long Wave Equation Using the Optimal Homotopy Perturbation Method

    Directory of Open Access Journals (Sweden)

    Constantin Bota

    2014-01-01

    Full Text Available The paper presents the optimal homotopy perturbation method, which is a new method to find approximate analytical solutions for nonlinear partial differential equations. Based on the well-known homotopy perturbation method, the optimal homotopy perturbation method presents an accelerated convergence compared to the regular homotopy perturbation method. The applications presented emphasize the high accuracy of the method by means of a comparison with previous results.

  2. Zinco eritrocitário (validação de um método de análise e zinco dietético na avaliação do estado nutricional de mulheres adultas Erythrocytic zinc (validation of an analytical method and dietetic in nutriture evaluation of adult women

    Directory of Open Access Journals (Sweden)

    Hosana Gonçalves dos Santos

    2005-06-01

    Full Text Available O objetivo deste estudo foi validar um método de determinação de zinco eritrocitário (ZnER por espectrofotometria de absorção atômica (EAA, avaliar com esse parâmetro o estado nutricional em Zn de mulheres adultas, relacioná-lo com a ingestão dietética diária, identificando os alimentos fonte do mineral. O método foi validado com limites de detecção e de quantificação de 0,006 e 0,045(0,013 migZn/mL, respectivamente, e níveis de exatidão e de imprecisão intra-ensaio e inter-ensaio de 95 (0,4% , 3,6% e 5,3%, respectivamente. A ingestão média de Zn do grupo (n=21 foi de 9,7(3mgZn/dia e 15 desses resultados estão acima da RDA de 8 mg/d e 4 abaixo da EAR de 6,8 mg/d (Institute of Medicine/2000b. A concentração média de ZnER foi de 38,2(5 mgZn/gHb, valor menor do que o encontrado por outros autores para o mesmo gênero e estágio de vida. As fontes de Zn da dieta do grupo (>1,2 mg Zn/100 g foram: carnes bovina e suína, fígado bovino, linguiça, queijos dos tipos prato, branco, gouda e mussarela e amendoim.The aim of this study was to validate a method for determining erythrocytic Zn (ZnER by atomic absorption spectrophotometry (AAS, in order to evaluate, with this parameter, the Zn nutriture of adult women (n=21, and to relate it with the dietary daily Zn ingestion by the group. The method was validated with limits of detection and quantification of 0.006 and 0.045(0.013mgZn/mL, respectively, and accuracy and intra and inter-assay coefficients of variation of 95(0.4%, 3.6% and 5.3%, respectively. The average daily ingestion of Zn by the adult women was 9.7(3mgZn/d, 15 of them had intake levels above the Recommended Dietary Allowance of 8 mg/d (RDA/2001 and 4 below the Estimated Average Requirement of 6,8 mg/d (EAR /2001. The average concentration of ZnER was 38.2(5 mgZn/gHb, a value lower than that found by other authors for the same age and gender group. Food sources of Zn in their diets (>1.2 mg Zn/serving were: bovine

  3. Ernst Equation and Riemann Surfaces: Analytical and Numerical Methods

    Energy Technology Data Exchange (ETDEWEB)

    Ernst, Frederick J [FJE Enterprises, 511 County Route 59, Potsdam, NY 13676 (United States)

    2007-06-18

    source can be represented by discontinuities in the metric tensor components. The first two chapters of this book are devoted to some basic ideas: in the introductory chapter 1 the authors discuss the concept of integrability, comparing the integrability of the vacuum Ernst equation with the integrability of nonlinear equations of Korteweg-de Vries (KdV) type, while in chapter 2 they describe various circumstances in which the vacuum Ernst equation has been determined to be relevant, not only in connection with gravitation but also, for example, in the construction of solutions of the self-dual Yang-Mills equations. It is also in this chapter that one of several equivalent linear systems for the Ernst equation is described. The next two chapters are devoted to Dmitry Korotkin's concept of algebro-geometric solutions of a linear system: in chapter 3 the structure of such solutions of the vacuum Ernst equation, which involve Riemann theta functions of hyperelliptic algebraic curves of any genus, is contrasted with the periodic structure of such solutions of the KdV equation. How such solutions can be obtained, for example, by solving a matrix Riemann-Hilbert problem and how the metric tensor of the associated spacetime can be evaluated is described in detail. In chapter 4 the asymptotic behaviour and the similarity structure of the general algebro-geometric solutions of the Ernst equation are described, and the relationship of such solutions to the perhaps more familiar multi-soliton solutions is discussed. The next three chapters are based upon the authors' own published research: in chapter 5 it is shown that a problem involving counter-rotating infinitely thin disks of matter can be solved in terms of genus two Riemann theta functions, while in chapter 6 the authors describe numerical methods that facilitate the construction of such solutions, and in chapter 7 three-dimensional graphs are displayed that depict all metrical fields of the associated spacetime

  4. Laboratory diagnostic methods, system of quality and validation

    Directory of Open Access Journals (Sweden)

    Ašanin Ružica

    2005-01-01

    Full Text Available It is known that laboratory investigations secure safe and reliable results that provide a final confirmation of the quality of work. Ideas, planning, knowledge, skills, experience, and environment, along with good laboratory practice, quality control and reliability of quality, make the area of biological investigations very complex. In recent years, quality control, including the control of work in the laboratory, is based on international standards and is used at that level. The implementation of widely recognized international standards, such as the International Standard ISO/IEC 17025 (1 and the implementing of the quality system series ISO/IEC 9000 (2 have become the imperative on the grounds of which laboratories have a formal, visible and corresponding system of quality. The diagnostic methods that are used must constantly yield results which identify the animal as positive or negative, and the precise status of the animal is determined with a predefined degree of statistical significance. Methods applied on a selected population reduce the risk of obtaining falsely positive or falsely negative results. A condition for this are well conceived and documented methods, with the application of the corresponding reagents, and work with professional and skilled staff. This process requires also a consistent implementation of the most rigorous experimental plans, epidemiological and statistical data and estimations, with constant monitoring of the validity of the applied methods. Such an approach is necessary in order to cut down the number of misconceptions and accidental mistakes, for a referent population of animals on which the validity of a method is tested. Once a valid method is included in daily routine investigations, it is necessary to apply constant monitoring for the purpose of internal quality control, in order adequately to evaluate its reproducibility and reliability. Consequently, it is necessary at least twice yearly to conduct

  5. Integrative Mixed Methods Data Analytic Strategies in Research on School Success in Challenging Circumstances

    Science.gov (United States)

    Jang, Eunice E.; McDougall, Douglas E.; Pollon, Dawn; Herbert, Monique; Russell, Pia

    2008-01-01

    There are both conceptual and practical challenges in dealing with data from mixed methods research studies. There is a need for discussion about various integrative strategies for mixed methods data analyses. This article illustrates integrative analytic strategies for a mixed methods study focusing on improving urban schools facing challenging…

  6. Waste Tank Organic Safety Program: Analytical methods development. Progress report, FY 1994

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, J.A.; Clauss, S.A.; Grant, K.E. [and others

    1994-09-01

    The objectives of this task are to develop and document extraction and analysis methods for organics in waste tanks, and to extend these methods to the analysis of actual core samples to support the Waste Tank organic Safety Program. This report documents progress at Pacific Northwest Laboratory (a) during FY 1994 on methods development, the analysis of waste from Tank 241-C-103 (Tank C-103) and T-111, and the transfer of documented, developed analytical methods to personnel in the Analytical Chemistry Laboratory (ACL) and 222-S laboratory. This report is intended as an annual report, not a completed work.

  7. Development and validation of a multi-analyte LC-MS/MS approach for quantification of neuroleptics in whole blood, plasma, and serum.

    Science.gov (United States)

    Montenarh, Deborah; Hopf, Markus; Maurer, Hans H; Schmidt, Peter; Ewald, Andreas H

    2016-10-01

    Based on a similar approach for quantification of antidepressants, benzodiazepines, and z-drugs, a liquid chromatography-tandem mass spectrometry (LC-MS/MS) multi-analyte approach with simple liquid-liquid extraction was extended for fast target screening and quantification of neuroleptics in whole blood, plasma, and serum. As this method is part of a multi-analyte procedure for over 100 analytes from different drug classes and as the extracts were additionally used in the authors' laboratory for gas chromatography-mass spectrometry (GC-MS) analysis, one universal stable-isotope-labelled internal standard (SIL-IS) was used to save time and resource. The method was validated with respect to international guidelines. For accuracy and precision, full calibration was performed with ranges from subtherapeutic to toxic concentrations. Selectivity problems could not be observed, but matrix effects ranged from 68 to 211% in all samples. For the low quality control (QC), recovery ranged from 32 to 112%, process efficiency from 31 to 165% and for the high QC recovery from 42 to 141%, process efficiency from 29 to 154%. In addition statistical data evaluation of the variances of the recovery, matrix effects, and process efficiency data between whole blood vs. plasma, whole blood vs. serum, and plasma vs. serum were done. The presented LC-MS/MS approach was applicable for selective detection of 33 neuroleptics as well as accurate and precise quantification of 25 neuroleptics in whole blood, 19 in plasma, and 17 in serum. More significant matrix effects (ME) for neuropletic drugs overall in plasma and serum as compared with whole blood were detected. Copyright © 2015 John Wiley & Sons, Ltd.

  8. Analytical and Clinical Validation of a Digital Sequencing Panel for Quantitative, Highly Accurate Evaluation of Cell-Free Circulating Tumor DNA.

    Directory of Open Access Journals (Sweden)

    Richard B Lanman

    Full Text Available Next-generation sequencing of cell-free circulating solid tumor DNA addresses two challenges in contemporary cancer care. First this method of massively parallel and deep sequencing enables assessment of a comprehensive panel of genomic targets from a single sample, and second, it obviates the need for repeat invasive tissue biopsies. Digital Sequencing™ is a novel method for high-quality sequencing of circulating tumor DNA simultaneously across a comprehensive panel of over 50 cancer-related genes with a simple blood test. Here we report the analytic and clinical validation of the gene panel. Analytic sensitivity down to 0.1% mutant allele fraction is demonstrated via serial dilution studies of known samples. Near-perfect analytic specificity (> 99.9999% enables complete coverage of many genes without the false positives typically seen with traditional sequencing assays at mutant allele frequencies or fractions below 5%. We compared digital sequencing of plasma-derived cell-free DNA to tissue-based sequencing on 165 consecutive matched samples from five outside centers in patients with stage III-IV solid tumor cancers. Clinical sensitivity of plasma-derived NGS was 85.0%, comparable to 80.7% sensitivity for tissue. The assay success rate on 1,000 consecutive samples in clinical practice was 99.8%. Digital sequencing of plasma-derived DNA is indicated in advanced cancer patients to prevent repeated invasive biopsies when the initial biopsy is inadequate, unobtainable for genomic testing, or uninformative, or when the patient's cancer has progressed despite treatment. Its clinical utility is derived from reduction in the costs, complications and delays associated with invasive tissue biopsies for genomic testing.

  9. Analytical and Clinical Validation of a Digital Sequencing Panel for Quantitative, Highly Accurate Evaluation of Cell-Free Circulating Tumor DNA.

    Science.gov (United States)

    Lanman, Richard B; Mortimer, Stefanie A; Zill, Oliver A; Sebisanovic, Dragan; Lopez, Rene; Blau, Sibel; Collisson, Eric A; Divers, Stephen G; Hoon, Dave S B; Kopetz, E Scott; Lee, Jeeyun; Nikolinakos, Petros G; Baca, Arthur M; Kermani, Bahram G; Eltoukhy, Helmy; Talasaz, AmirAli

    2015-01-01

    Next-generation sequencing of cell-free circulating solid tumor DNA addresses two challenges in contemporary cancer care. First this method of massively parallel and deep sequencing enables assessment of a comprehensive panel of genomic targets from a single sample, and second, it obviates the need for repeat invasive tissue biopsies. Digital Sequencing™ is a novel method for high-quality sequencing of circulating tumor DNA simultaneously across a comprehensive panel of over 50 cancer-related genes with a simple blood test. Here we report the analytic and clinical validation of the gene panel. Analytic sensitivity down to 0.1% mutant allele fraction is demonstrated via serial dilution studies of known samples. Near-perfect analytic specificity (> 99.9999%) enables complete coverage of many genes without the false positives typically seen with traditional sequencing assays at mutant allele frequencies or fractions below 5%. We compared digital sequencing of plasma-derived cell-free DNA to tissue-based sequencing on 165 consecutive matched samples from five outside centers in patients with stage III-IV solid tumor cancers. Clinical sensitivity of plasma-derived NGS was 85.0%, comparable to 80.7% sensitivity for tissue. The assay success rate on 1,000 consecutive samples in clinical practice was 99.8%. Digital sequencing of plasma-derived DNA is indicated in advanced cancer patients to prevent repeated invasive biopsies when the initial biopsy is inadequate, unobtainable for genomic testing, or uninformative, or when the patient's cancer has progressed despite treatment. Its clinical utility is derived from reduction in the costs, complications and delays associated with invasive tissue biopsies for genomic testing.

  10. Validation of high performance liquid chromatography method for determination of meloxicam loaded PEGylated nanocapsules

    Directory of Open Access Journals (Sweden)

    Francine Rodrigues Ianiski

    2015-12-01

    Full Text Available abstract A method to ensure that an analytical method will produce reliable and interpretable information about the sample must first be validated, making sure that the results can be trusted and traced. In this study, we propose to validate an analytical high performance liquid chromatography (HPLC method for the quantitation of meloxicam loaded PEGylated nanocapsules(M-PEGNC. We performed a validation study, evaluated parameters including specificity, linearity, quantification limit, detection limit, accuracy, precision and robustness. PEGylated nanocapsules were prepared by interfacial deposition of preformed polymer, and the particle size, polydispersity index, zeta potential, pH value and encapsulation efficiency were characterized. The proposed HPLC method provides selective, linear results in the range of 1.0-40.0 μg/mL; quantification and detection limits were 1.78 μg/mL and 0.59 μg/mL, respectively; relative standard deviation for repeatability was 1.35% and intermediate precision was 0.41% and 0.61% for analyst 1 and analyst 2, respectively; accuracy between 99.23 and 101.79%; robustness between 97.13 and 98.45% for the quantification of M-PEGNC. Mean particle diameters were 261 ± 13 nm and 249 ± 20 nm, polydispersity index was 0.15 ± 0.07 and 0.17 ± 0.06, pH values were 5.0 ± 0.2 and 5.2 ± 0.1, and zeta-potential values were -37.9 ± 3.2 mV e -31.8 ± 2.8 mV for M-PEGNC and placebo(B-PEGNC, respectively. In conclusion, the proposed analytical method is suitable for the quality control of M-PEGNC. Moreover, suspensions showed monomodal size distributions and low polydispersity index indicating high homogeneity of formulations with narrow size distributions, and appropriate pH and zeta potential. The extraction process was efficient for release of meloxicam from nanostructured systems.

  11. Mycotoxin and fungicide residues in wheat grains from fungicide-treated plants measured by a validated LC-MS method.

    Science.gov (United States)

    da Luz, Suzane Rickes; Pazdiora, Paulo Cesar; Dallagnol, Leandro José; Dors, Giniani Carla; Chaves, Fábio Clasen

    2017-04-01

    Wheat (Triticum aestivum) is an annual crop, cultivated in the winter and spring and susceptible to several pathogens, especially fungi, which are managed with fungicides. It is also one of the most consumed cereals, and can be contaminated by mycotoxins and fungicides. The objective of this study was to validate an analytical method by LC-MS for simultaneous determination of mycotoxins and fungicide residues in wheat grains susceptible to fusarium head blight treated with fungicides, and to evaluate the relationship between fungicide application and mycotoxin production. All parameters of the validated analytical method were within AOAC and ANVISA limits. Deoxynivalenol was the prevalent mycotoxin in wheat grain and epoxiconazole was the fungicide residue found in the highest concentration. All fungicidal treatments induced an increase in AFB2 production when compared to the control (without application). AFB1 and deoxynivalenol, on the contrary, were reduced in all fungicide treatments compared to the control.

  12. Validation of an analytical method for the determination of total mercury in urine samples using cold vapor atomic absorption spectrometry (CV-AAS); Validacao de metodologia analitica para determinacao de mercurio total em amostras de urina por espectrometria de absorcao atomica com geracao de vapor frio (CV-AAS)

    Energy Technology Data Exchange (ETDEWEB)

    Guilhen, Sabine Neusatz

    2009-07-01

    Mercury (Hg) is a toxic metal applied to a variety of products and processes, representing a risk to the health of occupationally or accidentally exposed subjects. Dental amalgam is a restorative material composed of metallic mercury, which use has been widely debated in the last decades. Due to the dubiety of the studies concerning dental amalgam, many efforts concerning this issue have been conducted. The Tropical Medicine Foundation (Tocantins, Brazil) has recently initiated a study to evaluate the environmental and occupational levels of exposure to mercury in dentistry attendants at public consulting rooms in the city of Araguaina (TO). In collaboration with this study, the laboratory of analysis at IPEN's Chemistry and Environment Center is undertaking the analysis of mercury levels in exposed subjects' urine samples using cold vapor atomic absorption spectrometry. This analysis requires the definition of a methodology capable of generating reliable results. Such methodology can only be implemented after a rigorous validation procedure. As part of this work, a series of tests were conducted in order to confirm the suitability of the selected methodology and to assert that the laboratory addresses all requirements needed for a successful implementation of the methodology. The following parameters were considered in order to test the method’s performance: detection and quantitation limits, selectivity, sensitivity, linearity, accuracy and precision. The assays were carried out with certified reference material, which assures the traceability of the results. Taking into account the estimated parameters, the method can be considered suitable for the afore mentioned purpose. The mercury concentration found for the reference material was of (95,12 ± 11,70)μg.L{sup -1} with a recovery rate of 97%. The method was also applied to 39 urine samples, six of which (15%) showing urinary mercury levels above the normal limit of 10μg.L{sup −1}. The obtained

  13. Application of Statistical Methods to Activation Analytical Results near the Limit of Detection

    DEFF Research Database (Denmark)

    Heydorn, Kaj; Wanscher, B.

    1978-01-01

    Reporting actual numbers instead of upper limits for analytical results at or below the detection limit may produce reliable data when these numbers are subjected to appropriate statistical processing. Particularly in radiometric methods, such as activation analysis, where individual standard...... deviations of analytical results may be estimated, improved discrimination may be based on the Analysis of Precision. Actual experimental results from a study of the concentrations of arsenic in human skin demonstrate the power of this principle....

  14. Analytical calculation of optimal POVM for unambiguous discrimination of quantum states using KKT method

    CERN Document Server

    Karimi, N

    2011-01-01

    In the present paper, an exact analytic solution for the optimal unambiguous state discrimination (OPUSD) problem involving an arbitrary number of pure linearly independent quantum states with real and complex inner product is presented. Using semidefinite programming and Karush-Kuhn-Tucker convex optimization method, we derive an analytical formula which shows the relation between optimal solution of unambiguous state discrimination problem and an arbitrary number of pure linearly independent quantum states.

  15. Analytic Solutions of Some Self-Adjoint Equations by Using Variable Change Method and Its Applications

    OpenAIRE

    Mehdi Delkhosh; Mohammad Delkhosh

    2012-01-01

    Many applications of various self-adjoint differential equations, whose solutions are complex, are produced (Arfken, 1985; Gandarias, 2011; and Delkhosh, 2011). In this work we propose a method for the solving some self-adjoint equations with variable change in problem, and then we obtain a analytical solutions. Because this solution, an exact analytical solution can be provided to us, we benefited from the solution of numerical Self-adjoint equations (Mohynl-Din, 2009; Allame and Azal, 2011;...

  16. Analytic Continuation in the Coupling Constant Method for the Dirac Equation

    Institute of Scientific and Technical Information of China (English)

    张时声; 郭建友; 张双全; 孟杰

    2004-01-01

    On the basis of the Dirac equation, the analytic continuation in the coupling constant method is employed to investigate the energies and widths of single-particle resonant in square-well, harmonic-oscillator, and Woodsconvergent energies and widths of single-particle resonant states can be obtained, which makes the application of the analytic continuation in the coupling constant for the relativistic mean field theory possible.

  17. Development of novel analytical methods to study the metabolism of coumarin

    OpenAIRE

    1996-01-01

    The research in this thesis revolves around developing analytical methods for the determination of coumann and 7-hydroxycoumann for various applications. The techniques used in this work were, capillary electrophoresis, immunosensing and electrochemistry. Chapter 1 serves as general review of the analysis of coumann and 7-hydroxycoumann, including the many different types of analytical technique which have been used to analyse this drug. Capillary electrophoresis was used as the basis of a me...

  18. Validation of thermodesorption method for analysis of semi-volatile organic compounds adsorbed on wafer surface.

    Science.gov (United States)

    Hayeck, Nathalie; Gligorovski, Sasho; Poulet, Irène; Wortham, Henri

    2014-05-01

    To prevent the degradation of the device characteristics it is important to detect the organic contaminants adsorbed on the wafers. In this respect, a reliable qualitative and quantitative analytical method for analysis of semi-volatile organic compounds which can adsorb on wafer surfaces is of paramount importance. Here, we present a new analytical method based on Wafer Outgassing System (WOS) coupled to Automated Thermal Desorber-Gas chromatography-Mass spectrometry (ATD-GC-MS) to identify and quantify volatile and semi-volatile organic compounds from 6", 8" and 12" wafers. WOS technique allows the desorption of organic compounds from one side of the wafers. This method was tested on three important airborne contaminants in cleanroom i.e. tris-(2-chloroethyl) phosphate (TCEP), tris-(2-chloroisopropyl) phosphate (TCPP) and diethyl phthalate (DEP). In addition, we validated this method for the analysis and quantification of DEP, TCEP and TCPP and we estimated the backside organic contamination which may contribute to the front side of the contaminated wafers. We are demonstrating that WOS/ATD-GC-MS is a suitable and highly efficient technique for desorption and quantitative analysis of organophosphorous compounds and phthalate ester which could be found on the wafer surface.

  19. Development and validation of an HPLC–MS/MS method to determine clopidogrel in human plasma

    Science.gov (United States)

    Liu, Gangyi; Dong, Chunxia; Shen, Weiwei; Lu, Xiaopei; Zhang, Mengqi; Gui, Yuzhou; Zhou, Qinyi; Yu, Chen

    2015-01-01

    A quantitative method for clopidogrel using online-SPE tandem LC–MS/MS was developed and fully validated according to the well-established FDA guidelines. The method achieves adequate sensitivity for pharmacokinetic studies, with lower limit of quantifications (LLOQs) as low as 10 pg/mL. Chromatographic separations were performed on reversed phase columns Kromasil Eternity-2.5-C18-UHPLC for both methods. Positive electrospray ionization in multiple reaction monitoring (MRM) mode was employed for signal detection and a deuterated analogue (clopidogrel-d4) was used as internal standard (IS). Adjustments in sample preparation, including introduction of an online-SPE system proved to be the most effective method to solve the analyte back-conversion in clinical samples. Pooled clinical samples (two levels) were prepared and successfully used as real-sample quality control (QC) in the validation of back-conversion testing under different conditions. The result showed that the real samples were stable in room temperature for 24 h. Linearity, precision, extraction recovery, matrix effect on spiked QC samples and stability tests on both spiked QCs and real sample QCs stored in different conditions met the acceptance criteria. This online-SPE method was successfully applied to a bioequivalence study of 75 mg single dose clopidogrel tablets in 48 healthy male subjects. PMID:26904399

  20. Development and validation of an HPLC–MS/MS method to determine clopidogrel in human plasma

    Directory of Open Access Journals (Sweden)

    Gangyi Liu

    2016-01-01

    Full Text Available A quantitative method for clopidogrel using online-SPE tandem LC–MS/MS was developed and fully validated according to the well-established FDA guidelines. The method achieves adequate sensitivity for pharmacokinetic studies, with lower limit of quantifications (LLOQs as low as 10 pg/mL. Chromatographic separations were performed on reversed phase columns Kromasil Eternity-2.5-C18-UHPLC for both methods. Positive electrospray ionization in multiple reaction monitoring (MRM mode was employed for signal detection and a deuterated analogue (clopidogrel-d4 was used as internal standard (IS. Adjustments in sample preparation, including introduction of an online-SPE system proved to be the most effective method to solve the analyte back-conversion in clinical samples. Pooled clinical samples (two levels were prepared and successfully used as real-sample quality control (QC in the validation of back-conversion testing under different conditions. The result showed that the real samples were stable in room temperature for 24 h. Linearity, precision, extraction recovery, matrix effect on spiked QC samples and stability tests on both spiked QCs and real sample QCs stored in different conditions met the acceptance criteria. This online-SPE method was successfully applied to a bioequivalence study of 75 mg single dose clopidogrel tablets in 48 healthy male subjects.

  1. Spectrophotometric validation of assay method for selected medicinal plant extracts

    Directory of Open Access Journals (Sweden)

    Matthew Arhewoh

    2014-09-01

    Full Text Available Objective: To develop UV spectrophotometric assay validation methods for some selected medicinal plant extracts.Methods: Dried, powdered leaves of Annona muricata (AM and Andrographis paniculata (AP as well as seeds of Garcinia kola (GK and Hunteria umbellata (HU were separately subjected to maceration using distilled water. Different concentrations of the extracts were scanned spectrophotometrically to obtain wavelengths of maximum absorbance. The different extracts were then subjected to validation studies following international guidelines at the respective wavelengths obtained.Results: The results showed linearity at peak wavelengths of maximum absorbance of 292, 280, 274 and 230 nm for GK, HU, AM and AP, respectively. The calibration curves for the different concentrations of the extract gave R2 values ranging from 0.9831 for AM to 0.9996 for AP the inter-day and intra-day precision study showed that the relative standard deviation (% was ≤ 10% for all the extracts.Conclusion: The aqueous extracts and isolates of these plants can be assayed and monitored using these wavelengths.

  2. A retrieval and validation method for shelterbelt vegetation fraction

    Institute of Scientific and Technical Information of China (English)

    DENG Rong-xin; WANG Wen-juan; LI Ying; ZHAO Dong-bao

    2013-01-01

    Shelterbelts are important in defending against natural disaster and maintaining ecological balances in farmland.Understanding of the shelterbelt vegetation fraction is fundamental to regional research of shelterbelts using remote sensing.We used SPOT5 imagery with 10×10m spatial resolution in combination with knowledge of the characteristics of shelterbelts to develop a method for retrieval of the vegetation fraction of shelterbelts by the pixel un-mixing model.We then used the method to retrieve values for shelterbelts in study area.By combining the parameters of photographic images with characteristics of shelterbelts,we developed a method for measuring the vegetation fraction of shelterbelts based on an advanced photographic method.We then measured the actual values to validate the retrieval result.The multiple correlation coefficients between the retrieved and measured values were 0.715.Our retrieval and measuring methods presented in this paper accurately reflect field conditions.We suggest that this method is useful to describe shelterbelt structure using remote sensing.

  3. Video quality experts group: the quest for valid objective methods

    Science.gov (United States)

    Corriveau, Philip J.; Webster, Arthur A.; Rohaly, Ann M.; Libert, John M.

    2000-06-01

    Subjective assessment methods have been used reliably for many years to evaluate video quality. They continue to provide the most reliable assessments compared to objective methods. Some issues that arise with subjective assessment include the cost of conducting the evaluations and the fact that these methods cannot easily be used to monitor video quality in real time. Furthermore, traditional, analog objective methods, while still necessary, are not sufficient to measure the quality of digitally compressed video systems. Thus, there is a need to develop new objective methods utilizing the characteristics of the human visual system. While several new objective methods have been developed, there is to date no internationally standardized method. The Video Quality Experts Group (VQEG) was formed in October 1997 to address video quality issues. The group is composed of experts from various backgrounds and affiliations, including participants from several internationally recognized organizations working in the field of video quality assessment. The majority of participants are active in the International Telecommunications Union (ITU) and VQEG combines the expertise and resources found in several ITU Study Groups to work towards a common goal. The first task undertaken by VQEG was to provide a validation of objective video quality measurement methods leading to Recommendations in both the Telecommunications (ITU-T) and Radiocommunication (ITU-R) sectors of the ITU. To this end, VQEG designed and executed a test program to compare subjective video quality evaluations to the predictions of a number of proposed objective measurement methods for video quality in the bit rate range of 768 kb/s to 50 Mb/s. The results of this test show that there is no objective measurement system that is currently able to replace subjective testing. Depending on the metric used for evaluation, the performance of eight or nine models was found to be statistically equivalent, leading to the

  4. Validity of the small-amplitude limit of the nuclear Born-Oppenheimer method

    Energy Technology Data Exchange (ETDEWEB)

    Zettili, Nouredine (Department of Physics, King Fahd University of Petroleum and Minerals, Dhahran, 31261 (Saudi Arabia) Institut de Physique, Universite de Blida, Blida (Algeria))

    1994-08-22

    We examine here the validity of the small-amplitude limit of the nuclear Born-Oppenheimer (NBO) method by testing it on an analytically solvable model. To gain additional quantitative insight into its accuracy, we provide a comparison of its results with those of the small-amplitude limit of the time-dependent Hartree-Fock (TDHF) when applied to this model. A comparison of the exact, the random-phase approximation (RPA), and the NBO results reveals that the NBO energy is lower than its RPA counterpart and is in very good agreement with the exact spectrum. We also provide a quantitative assessment of the effects the approximations involved in the NBO method have on the results. We show that, when corrections to these approximations are considered, the NBO energy spectrum becomes much more accurate. ((orig.))

  5. Validity of the small-amplitude limit of the nuclear Born-Oppenheimer method

    Science.gov (United States)

    Zettili, Nouredine

    1994-08-01

    We examine here the validity of the small-amplitude limit of the nuclear Born-Op-penheimer (NBO) method by testing it on an analytically solvable model. To gain additional quantitative insight into its accuracy, we provide a comparison of its results with those of the small-amplitude limit of the time-dependent Hartree-Fock (TDHF) when applied to this model. A comparison of the exact, the random-phase approximation (RPA), and the NBO results reveals that the NBO energy is lower than its RPA counterpart and is in very good agreement with the exact spectrum. We also provide a quantitative assessment of the effects the approximations involved in the NBO method have on the results. We show that, when corrections to these approximations are considered, the NBO energy spectrum becomes much more accurate.

  6. Selenium contaminated waters: An overview of analytical methods, treatment options and recent advances in sorption methods.

    Science.gov (United States)

    Santos, Sílvia; Ungureanu, Gabriela; Boaventura, Rui; Botelho, Cidália

    2015-07-15

    Selenium is an essential trace element for many organisms, including humans, but it is bioaccumulative and toxic at higher than homeostatic levels. Both selenium deficiency and toxicity are problems around the world. Mines, coal-fired power plants, oil refineries and agriculture are important examples of anthropogenic sources, generating contaminated waters and wastewaters. For reasons of human health and ecotoxicity, selenium concentration has to be controlled in drinking-water and in wastewater, as it is a potential pollutant of water bodies. This review article provides firstly a general overview about selenium distribution, sources, chemistry, toxicity and environmental impact. Analytical techniques used for Se determination and speciation and water and wastewater treatment options are reviewed. In particular, published works on adsorption as a treatment method for Se removal from aqueous solutions are critically analyzed. Recent published literature has given particular attention to the development and search for effective adsorbents, including low-cost alternative materials. Published works mostly consist in exploratory findings and laboratory-scale experiments. Binary metal oxides and LDHs (layered double hydroxides) have presented excellent adsorption capacities for selenium species. Unconventional sorbents (algae, agricultural wastes and other biomaterials), in raw or modified forms, have also led to very interesting results with the advantage of their availability and low-cost. Some directions to be considered in future works are also suggested.

  7. Analytical method for reconstruction pin to pin of the nuclear power density distribution

    Energy Technology Data Exchange (ETDEWEB)

    Pessoa, Paulo O.; Silva, Fernando C.; Martinez, Aquilino S., E-mail: ppessoa@con.ufrj.br, E-mail: fernando@con.ufrj.br, E-mail: aquilino@imp.ufrj.br [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil)

    2013-07-01

    An accurate and efficient method for reconstructing pin to pin of the nuclear power density distribution, involving the analytical solution of the diffusion equation for two-dimensional neutron energy groups in homogeneous nodes, is presented. The boundary conditions used for analytic as solution are the four currents or fluxes on the surface of the node, which are obtained by Nodal Expansion Method (known as NEM) and four fluxes at the vertices of a node calculated using the finite difference method. The analytical solution found is the homogeneous distribution of neutron flux. Detailed distributions pin to pin inside a fuel assembly are estimated by the product of homogeneous flux distribution by local heterogeneous form function. Furthermore, the form functions of flux and power are used. The results obtained with this method have a good accuracy when compared with reference values. (author)

  8. MULTIPLE CRITERA METHODS WITH FOCUS ON ANALYTIC HIERARCHY PROCESS AND GROUP DECISION MAKING

    Directory of Open Access Journals (Sweden)

    Lidija Zadnik-Stirn

    2010-12-01

    Full Text Available Managing natural resources is a group multiple criteria decision making problem. In this paper the analytic hierarchy process is the chosen method for handling the natural resource problems. The one decision maker problem is discussed and, three methods: the eigenvector method, data envelopment analysis method, and logarithmic least squares method are presented for the derivation of the priority vector. Further, the group analytic hierarchy process is discussed and six methods for the aggregation of individual judgments or priorities: weighted arithmetic mean method, weighted geometric mean method, and four methods based on data envelopment analysis are compared. The case study on land use in Slovenia is applied. The conclusions review consistency, sensitivity analyses, and some future directions of research.

  9. OPTIMAL METHOD FOR PREPARATION OF SILICATE ROCK SAMPLES FOR ANALYTICAL PURPOSES

    Directory of Open Access Journals (Sweden)

    Maja Vrkljan

    2004-12-01

    Full Text Available The purpose of this study was to determine an optimal dissolution method for silicate rock samples for further analytical purposes. Analytical FAAS method of determining cobalt, chromium, copper, nickel, lead and zinc content in gabbro sample and geochemical standard AGV-1 has been applied for verification. Dissolution in mixtures of various inorganic acids has been tested, as well as Na2CO3 fusion technique. The results obtained by different methods have been compared and dissolution in the mixture of HNO3 + HF has been recommended as optimal.

  10. A method based on stochastic resonance for the detection of weak analytical signal.

    Science.gov (United States)

    Wu, Xiaojing; Guo, Weiming; Cai, Wensheng; Shao, Xueguang; Pan, Zhongxiao

    2003-12-23

    An effective method for detection of weak analytical signals with strong noise background is proposed based on the theory of stochastic resonance (SR). Compared with the conventional SR-based algorithms, the proposed algorithm is simplified by changing only one parameter to realize the weak signal detection. Simulation studies revealed that the method performs well in detection of analytical signals in very high level of noise background and is suitable for detecting signals with the different noise level by changing the parameter. Applications of the method to experimental weak signals of X-ray diffraction and Raman spectrum are also investigated. It is found that reliable results can be obtained.

  11. Comparison of the traditional pharmaceutical validation method versus an assisted pharmaceutical validation in hospitalized patients

    Directory of Open Access Journals (Sweden)

    D. García Marco

    2016-05-01

    Full Text Available Objective: To analyze pharmaceutical interventions that have been carried out with the support of an automated system for validation of treatments vs. the traditional method without computer support. Method: The automated program, ALTOMEDICAMENTOS® version 0, has 925 052 data with information regarding approximately 20 000 medicines, analyzing doses, administration routes, number of days with such a treatment, dosing in renal and liver failure, interactions control, similar drugs, and enteral medicines. During eight days, in four different hospitals (high complexity with over 1 000 beds, 400-bed intermediate, geriatric and monographic, the same patients and treatments were analyzed using both systems. Results: 3,490 patients were analyzed, with 42 155 different treatments. 238 interventions were performed using the traditional system (interventions 0.56% / possible interventions vs. 580 (1.38% with the automated one. Very significant pharmaceutical interventions were 0.14% vs. 0.46%; significant was 0.38% vs. 0.90%; non-significant was 0.05% vs. 0.01%, respectively. If both systems are simultaneously used, interventions are performed in 1.85% vs. 0.56% with just the traditional system. Using only the traditional model, 30.5% of the possible interventions are detected, whereas without manual review and only the automated one, 84% of the possible interventions are detected. Conclusions: The automated system increases pharmaceutical interventions between 2.43 to 3.64 times. According to the results of this study the traditional validation system needs to be revised relying on automated systems. The automated program works correctly in different hospitals

  12. Validation of internal dosimetry protocols based on stochastic method

    Energy Technology Data Exchange (ETDEWEB)

    Mendes, Bruno M.; Fonseca, Telma C.F., E-mail: bmm@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil); Almeida, Iassudara G.; Trindade, Bruno M.; Campos, Tarcisio P.R., E-mail: tprcampos@yahoo.com.br [Universidade Federal de Minas Gerais (DEN/UFMG), Belo Horizonte, MG (Brazil). Departamento de Engenharia Nuclear

    2015-07-01

    Computational phantoms adapted to Monte Carlo codes have been applied successfully in radiation dosimetry fields. NRI research group has been developing Internal Dosimetry Protocols - IDPs, addressing distinct methodologies, software and computational human-simulators, to perform internal dosimetry, especially for new radiopharmaceuticals. Validation of the IDPs is critical to ensure the reliability of the simulations results. Inter comparisons of data from literature with those produced by our IDPs is a suitable method for validation. The aim of this study was to validate the IDPs following such inter comparison procedure. The Golem phantom has been reconfigured to run on MCNP5. The specific absorbed fractions (SAF) for photon at 30, 100 and 1000 keV energies were simulated based on the IDPs and compared with reference values (RV) published by Zankl and Petoussi-Henss, 1998. The SAF average differences from RV and those obtained in IDP simulations was 2.3 %. The SAF largest differences were found in situations involving low energy photons at 30 keV. The Adrenals and thyroid, i.e. the lowest mass organs, had the highest SAF discrepancies towards RV as 7.2 % and 3.8 %, respectively. The statistic differences of SAF applying our IDPs from reference values were considered acceptable at the 30, 100 and 1000 keV spectra. We believe that the main reason for the discrepancies in IDPs run, found in lower masses organs, was due to our source definition methodology. Improvements of source spatial distribution in the voxels may provide outputs more consistent with reference values for lower masses organs. (author)

  13. Determination of nifuroxazide and drotaverine hydrochloride in pharmaceutical preparations by three independent analytical methods.

    Science.gov (United States)

    Metwally, Fadia H; Abdelkawy, Mohammed; Naguib, Ibrahim A

    2006-01-01

    Three new, different, simple, sensitive, and accurate methods were developed for quantitative determination of nifuroxazide (I) and drotaverine hydrochloride (II) in a binary mixture. The first method was spectrophotometry, which allowed determination of I in the presence of II using a zero-order spectrum with an analytically useful maximum at 364.5 nm that obeyed Beer's law over a concentration range of 2-10 microg/mL with mean percentage recovery of 100.08 +/- 0.61. Determination of II in presence of I was obtained by second derivative spectrophotometry at 243.6 nm, which obeyed Beer's law over a concentration range of 2-10 microg/mL with mean recovery of 99.82 +/- 1.46%. The second method was spectrodensitometry, with which both drugs were separated on a silica gel plate using chloroform-acetone-methanol-glacial acetic acid (6 + 3 + 0.9 + 0.1) as the mobile phase and ultraviolet (UV) detection at 365 nm over a concentration range of 0.2-1 microg/band for both drugs, with mean recoveries of 99.99 +/- 0.15 and 100.00 +/- 0.34% for I and II, respectively. The third method was reversed-phase liquid chromatography using acetonitrile-water (40 + 60, v/v; adjusted to pH 2.55 with orthophosphoric acid) as the mobile phase and pentoxifylline as the internal standard at a flow rate of 1 mU/min with UV detection at 285 nm at ambient temperature over a concentration range of 2-10 microg/mL for both drugs, with mean recoveries of 100.24 +/- 1.51 and 100.08 +/- 0.78% for I and II, respectively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulations containing the above drugs with no interference from other dosage form additives. The validity of the suggested procedures was further assessed by applying the standard addition technique which was found to be satisfactory, and the percentage recoveries obtained were in accordance with those given by the EVA Pharma reference

  14. Rapid and alternative fabrication method for microfluidic paper based analytical devices.

    Science.gov (United States)

    Malekghasemi, Soheil; Kahveci, Enver; Duman, Memed

    2016-10-01

    A major application of microfluidic paper-based analytical devices (µPADs) includes the field of point-of-care (POC) diagnostics. It is important for POC diagnostics to possess properties such as ease-of-use and low cost. However, µPADs need multiple instruments and fabrication steps. In this study, two different chemicals (Hexamethyldisilazane and Tetra-ethylorthosilicate) were used, and three different methods (heating, plasma treatment, and microwave irradiation) were compared to develop µPADs. Additionally, an inkjet-printing technique was used for generating a hydrophilic channel and printing certain chemical agents on different regions of a modified filter paper. A rapid and effective fabrication method to develop µPADs within 10min was introduced using an inkjet-printing technique in conjunction with a microwave irradiation method. Environmental scanning electron microscope (ESEM) and x-ray photoelectron spectroscopy (XPS) were used for morphology characterization and determining the surface chemical compositions of the modified filter paper, respectively. Contact angle measurements were used to fulfill the hydrophobicity of the treated filter paper. The highest contact angle value (141°±1) was obtained using the microwave irradiation method over a period of 7min, when the filter paper was modified by TEOS. Furthermore, by using this method, the XPS results of TEOS-modified filter paper revealed Si2p (23%) and Si-O bounds (81.55%) indicating the presence of Si-O-Si bridges and Si(OEt) groups, respectively. The ESEM results revealed changes in the porous structures of the papers and decreases in the pore sizes. Washburn assay measurements tested the efficiency of the generated hydrophilic channels in which similar water penetration rates were observed in the TEOS-modified filter paper and unmodified (plain) filter paper. The validation of the developed µPADs was performed by utilizing the rapid urease test as a model test system. The detection limit of

  15. Analytical solution of population balance equation involving aggregation and breakage in terms of auxiliary equation method

    Indian Academy of Sciences (India)

    Zehra Pinar; Abhishek Dutta; Guido Bény; Turgut Öziş

    2015-01-01

    This paper presents an effective analytical simulation to solve population balance equation (PBE), involving particulate aggregation and breakage, by making use of appropriate solution(s) of associated complementary equation via auxiliary equation method (AEM). Travelling wave solutions of the complementary equation of a nonlinear PBE with appropriately chosen parameters is taken to be analogous to the description of the dynamic behaviour of the particulate processes. For an initial proof-of-concept, a general case when the number of particles varies with respect to time is chosen. Three cases, i.e. (1) balanced aggregation and breakage, (2) when aggregation can dominate and (3) breakage can dominate, are selected and solved for their corresponding analytical solutions. The results are then compared with the available analytical solution, based on Laplace transform obtained from literature. In this communication, it is shown that the solution approach proposed via AEM is flexible and therefore more efficient than the analytical approach used in the literature.

  16. System and Method for Providing a Climate Data Analytic Services Application Programming Interface Distribution Package

    Science.gov (United States)

    Schnase, John L. (Inventor); Duffy, Daniel Q. (Inventor); Tamkin, Glenn S. (Inventor)

    2016-01-01

    A system, method and computer-readable storage devices for providing a climate data analytic services application programming interface distribution package. The example system can provide various components. The system provides a climate data analytic services application programming interface library that enables software applications running on a client device to invoke the capabilities of a climate data analytic service. The system provides a command-line interface that provides a means of interacting with a climate data analytic service by issuing commands directly to the system's server interface. The system provides sample programs that call on the capabilities of the application programming interface library and can be used as templates for the construction of new client applications. The system can also provide test utilities, build utilities, service integration utilities, and documentation.

  17. Validated spectrofluorometric methods for determination of amlodipine besylate in tablets

    Science.gov (United States)

    Abdel-Wadood, Hanaa M.; Mohamed, Niveen A.; Mahmoud, Ashraf M.

    2008-08-01

    Two simple and sensitive spectrofluorometric methods have been developed and validated for determination of amlodipine besylate (AML) in tablets. The first method was based on the condensation reaction of AML with ninhydrin and phenylacetaldehyde in buffered medium (pH 7.0) resulting in formation of a green fluorescent product, which exhibits excitation and emission maxima at 375 and 480 nm, respectively. The second method was based on the reaction of AML with 7-chloro-4-nitro-2,1,3-benzoxadiazole (NBD-Cl) in a buffered medium (pH 8.6) resulting in formation of a highly fluorescent product, which was measured fluorometrically at 535 nm ( λex, 480 nm). The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9949-0.9997) were found between the fluorescence intensity and the concentrations of AML in the concentration range of 0.35-1.8 and 0.55-3.0 μg ml -1 for ninhydrin and NBD-Cl methods, respectively. The limits of assays detection were 0.09 and 0.16 μg ml -1 for the first and second method, respectively. The precisions of the methods were satisfactory; the relative standard deviations were ranged from 1.69 to 1.98%. The proposed methods were successfully applied to the analysis of AML in pure and pharmaceutical dosage forms with good accuracy; the recovery percentages ranged from 100.4-100.8 ± 1.70-2.32%. The results were compared favorably with those of the reported method.

  18. Contextual and Analytic Qualities of Research Methods Exemplified in Research on Teaching

    Science.gov (United States)

    Svensson, Lennart; Doumas, Kyriaki

    2013-01-01

    The aim of the present article is to discuss contextual and analytic qualities of research methods. The arguments are specified in relation to research on teaching. A specific investigation is used as an example to illustrate the general methodological approach. It is argued that research methods should be carefully grounded in an understanding of…

  19. Flammable gas safety program. Analytical methods development: FY 1994 progress report

    Energy Technology Data Exchange (ETDEWEB)

    Campbell, J.A.; Clauss, S.; Grant, K.; Hoopes, V.; Lerner, B.; Lucke, R.; Mong, G.; Rau, J.; Wahl, K.; Steele, R.

    1994-09-01

    This report describes the status of developing analytical methods to account for the organic components in Hanford waste tanks, with particular focus on tanks assigned to the Flammable Gas Watch List. The methods that have been developed are illustrated by their application to samples obtained from Tank 241-SY-101 (Tank 101-SY).

  20. Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar$

    Institute of Scientific and Technical Information of China (English)

    Emilia Sawicki; Michel J. Hillebrand; Hilde Rosing; Jan H.M. Schellens; Bastiaan Nuijen; Jos H. Beijnen

    2016-01-01

    Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are sub-strates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chro-matographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

  1. Validation of a liquid chromatographic method for the pharmaceutical quality control of products containing elacridar

    Directory of Open Access Journals (Sweden)

    Emilia Sawicki

    2016-08-01

    Full Text Available Many anticancer drugs have an impaired bioavailability and poor brain penetration because they are substrates to drug efflux pumps such as P-glycoprotein and Breast Cancer Resistance Protein. Elacridar is a strong inhibitor of these two drug efflux pumps and therefore has great potential to improve oral absorption and brain penetration of many anticancer drugs. Currently, a clinical formulation of elacridar is unavailable and therefore the pharmaceutical development of a drug product is highly warranted. This also necessitates the availability of an analytical method for its quality control. A reverse-phase high-performance liquid chromatographic method with ultraviolet detection was developed for the pharmaceutical quality control of products containing elacridar as the active pharmaceutical ingredient. The analytical method was validated for linearity, accuracy, precision, selectivity, carry-over, stability of stock and reference solutions, stability of the final extract, stability-indicating capability and impurity testing. We found that elacridar is unstable in aqueous solutions that are exposed to light because a hydroxylation product of elacridar is formed. Therefore, sample solutions with elacridar must be protected from light.

  2. Validação de um método analítico para a determinação de substâncias ativas em formulações farmacêuticas empregadas em "peelings" químicos Validation of analytical methods for the determination of active substances in pharmaceutical preparations used in chemical peelings

    Directory of Open Access Journals (Sweden)

    Tatiane Rodrigues Ramos

    2005-06-01

    Full Text Available Nos "peelings" químicos utilizam-se formulações esfoliantes, empregadas na terapêutica de queratoses actínicas, rugas, discromias pigmentares, acne vulgar e rosácea. Na presente pesquisa, foram empregadas como amostras, a solução de Jessner (SJ composta por resorcinol (RS 14%, ácido salicílico (AS 14% e ácido láctico (AL 14% em solução alcoólica e géis de AS a 20% e RS a 30%. As técnicas utilizadas foram a espectrofotometria derivada no UV de primeira e segunda ordens em etanol absoluto para o AS e RS, respectivamente na SJ, e a espectrofotometria derivada no UV de primeira ordem em ácido sulfúrico 0,1 N para o AS e RS nos géis. Para o AS na SJ, o coeficiente de correlação (r foi de 0,9999, a precisão expressa pela média dos desvios padrão relativos (DPR de 0,68% e a exatidão expressa pela recuperação média de 100,5%. Para o RS na SJ o r foi de 0,9999, a média dos DPR de 0,83% e a recuperação média de 100,3%. No gel de AS, o r foi de 0,9999, a média dos DPR de 0,28 e a recuperação média de 99,3%. No gel de RS, o r foi de 0,9998, a média dos DPR de 0,34 e a recuperação média de 99,9%.Chemical peeling is obtained with exfoliating formulations and is used in the treatment of actinic keratosis, wrinkles, dyschromies, acne vulgaris and rosacea acne. In this research we selected the Jessner Solution (JS, a pharmaceutical preparation composed of resorcinol (RS (14%, salicylic acid (SA (14% and lactic acid (LA (14% in alcoholic solution and two gel samples composed of RS (30% and SA (20%, respectively. First and second derivative UV spectrophotometric methods were developed and validated for determination of SA and RS, respectively in JS alcoholic solution, ethanol was used as background. A first derivative UV spectrophotometric method was developed for determination of these active substances in gel samples using 0.1N sulfuric acid as background. For SA in the JS, the correlation coefficient (r was 0.9999, the

  3. Protein structure validation using a semi-empirical method

    Science.gov (United States)

    Lahiri, Tapobrata; Singh, Kalpana; Pal, Manoj Kumar; Verma, Gaurav

    2012-01-01

    Current practice of validating predicted protein structural model is knowledge-based where scoring parameters are derived from already known structures to obtain decision on validation out of this structure information. For example, the scoring parameter, Ramachandran Score gives percentage conformity with steric-property higher value of which implies higher acceptability. On the other hand, Force-Field Energy Score gives conformity with energy-wise stability higher value of which implies lower acceptability. Naturally, setting these two scoring parameters as target objectives sometimes yields a set of multiple models for the same protein for which acceptance based on a particular parameter, say, Ramachandran score, may not satisfy well with the acceptance of the same model based on other parameter, say, energy score. The confusion set of such models can further be resolved by introducing some parameters value of which are easily obtainable through experiment on the same protein. In this piece of work it was found that the confusion regarding final acceptance of a model out of multiple models of the same protein can be removed using a parameter Surface Rough Index which can be obtained through semi-empirical method from the ordinary microscopic image of heat denatured protein. PMID:23275692

  4. DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC ESTIMATION OF EBASTINE IN BULK AND TABLET DOSAGE FORM USING AREA UNDER CURVE METHOD

    Directory of Open Access Journals (Sweden)

    Dahivadkar Manish Sudhakar

    2013-06-01

    Full Text Available The aim of this work is to develop a simple, accurate, reproducible and cost effective spectrophotometric method for determination of Ebastine in bulk and pharmaceutical dosage form. This method is basedon area under curve (AUC in wavelength range of 247-257nm and method has followed linearity in the concentration range of 5-30μg/ml. Methanol was used as a solvent. The developed analytical method was validated as per International Conference on Harmonization (ICH guidelines. The value of correlation coefficient (R2 was 0.999. Limit of Detection and Limit of Quantitation were calculated as 0.78µg/ml and 2.37µg/ml, respectively. Results of the recovery studies showed good accuracy of the method. Validation results suggest that the developed method can be used for routine quality control studies for assay of Ebastine in bulk and tablet dosage form.

  5. Development of CAD implementing the algorithm of boundary elements’ numerical analytical method

    Directory of Open Access Journals (Sweden)

    Yulia V. Korniyenko

    2015-03-01

    Full Text Available Up to recent days the algorithms for numerical-analytical boundary elements method had been implemented with programs written in MATLAB environment language. Each program had a local character, i.e. used to solve a particular problem: calculation of beam, frame, arch, etc. Constructing matrices in these programs was carried out “manually” therefore being time-consuming. The research was purposed onto a reasoned choice of programming language for new CAD development, allows to implement algorithm of numerical analytical boundary elements method and to create visualization tools for initial objects and calculation results. Research conducted shows that among wide variety of programming languages the most efficient one for CAD development, employing the numerical analytical boundary elements method algorithm, is the Java language. This language provides tools not only for development of calculating CAD part, but also to build the graphic interface for geometrical models construction and calculated results interpretation.

  6. Review of Properties and Analytical Methods for the Determination of Norfloxacin.

    Science.gov (United States)

    Chierentin, Lucas; Salgado, Hérida Regina Nunes

    2016-01-01

    The first-generation quinolones have their greatest potency against Gram-negative bacteria, but newly developed molecules have exhibited increased potency against Gram-positive bacteria, and existing agents are available with additional activity against anaerobic microorganisms. Norfloxacin is a broad-spectrum antimicrobial fluoroquinolone used against Gram-positive and Gram-negative organisms (aerobic organisms). There are different analytical methods available to determine norfloxacin applied in quality control of this medicine in order to ensure its effectiveness and safety. The authors present an overview of the fourth generation of quinolones, followed by the properties, applications, and analytical methods of norfloxacin. These results show several existing analytical techniques that are flexible and broad-based methods of analysis in different matrices. This article focuses on bionalytical and pharmaceutical quality-control applications, such as thin-layer chromatography, microbiological assay, spectrophotometry, capillary electrophoresis (CE), and high-performance liquid chromatography (HPLC).

  7. Exploring valid and reliable assessment methods for care management education.

    Science.gov (United States)

    Gennissen, Lokke; Stammen, Lorette; Bueno-de-Mesquita, Jolien; Wieringa, Sietse; Busari, Jamiu

    2016-07-04

    Purpose It is assumed that the use of valid and reliable assessment methods can facilitate the development of medical residents' management and leadership competencies. To justify this assertion, the perceptions of an expert panel of health care leaders were explored on assessment methods used for evaluating care management (CM) development in Dutch residency programs. This paper aims to investigate how assessors and trainees value these methods and examine for any inherent benefits or shortcomings when they are applied in practice. Design/methodology/approach A Delphi survey was conducted among members of the platform for medical leadership in The Netherlands. This panel of experts was made up of clinical educators, practitioners and residents interested in CM education. Findings Of the respondents, 40 (55.6 per cent) and 31 (43 per cent) participated in the first and second rounds of the Delphi survey, respectively. The respondents agreed that assessment methods currently being used to measure residents' CM competencies were weak, though feasible for use in many residency programs. Multi-source feedback (MSF, 92.1 per cent), portfolio/e-portfolio (86.8 per cent) and knowledge testing (76.3 per cent) were identified as the most commonly known assessment methods with familiarity rates exceeding 75 per cent. Practical implications The findings suggested that an "assessment framework" comprising MSF, portfolios, individual process improvement projects or self-reflections and observations in clinical practice should be used to measure CM competencies in residents. Originality/value This study reaffirms the need for objective methods to assess CM skills in post-graduate medical education, as there was not a single assessment method that stood out as the best instrument.

  8. On the relationship between the causal-inference and meta-analytic paradigms for the validation of surrogate endpoints.

    Science.gov (United States)

    Alonso, Ariel; Van der Elst, Wim; Molenberghs, Geert; Buyse, Marc; Burzykowski, Tomasz

    2015-03-01

    The increasing cost of drug development has raised the demand for surrogate endpoints when evaluating new drugs in clinical trials. However, over the years, it has become clear that surrogate endpoints need to be statistically evaluated and deemed valid, before they can be used as substitutes of "true" endpoints in clinical studies. Nowadays, two paradigms, based on causal-inference and meta-analysis, dominate the scene. Nonetheless, although the literature emanating from these paradigms is wide, till now the relationship between them has largely been left unexplored. In the present work, we discuss the conceptual framework underlying both approaches and study the relationship between them using theoretical elements and the analysis of a real case study. Furthermore, we show that the meta-analytic approach can be embedded within a causal-inference framework on the one hand and that it can be heuristically justified why surrogate endpoints successfully evaluated using this approach will often be appealing from a causal-inference perspective as well, on the other. A newly developed and user friendly R package Surrogate is provided to carry out the evaluation exercise.

  9. Subsonic Indicial Aerodynamics for Aerofoil's Unsteady Loads via Numerical and Analytical Methods

    CERN Document Server

    Berci, Marco

    2016-01-01

    This study deals with generating aerodynamic indicial-admittance functions for predicting the unsteady lift of two-dimensional aerofoils in subsonic flow, using approximate numerical and analytical formulations. Both a step-change in the angle of attack and a sharp-edge gust are suitably considered as small perturbations. Novel contributions concern both a systematic analysis of the computational simulations process and an effective theoretical synthesis of its outcome, providing with sound cross-validation. Good practice for generating the indicial-admittance functions via computational fluid dynamics is first investigated for several Mach numbers, angles of attack and aerofoil profiles. Convenient analytical approximations of such indicial functions are then obtained by generalising those available for incompressible flow, taking advantage of acoustic wave theory for the non-circulatory airload and Prandtl-Glauert's scalability rule for the circulatory airload. An explicit parametric formula is newly propos...

  10. Development of a solvent-free analytical method for paracetamol quantitative determination in Blood Brain Barrier in vitro model.

    Science.gov (United States)

    Langlois, Marie-Hélène; Vekris, Antonios; Bousses, Christine; Mordelet, Elodie; Buhannic, Nathalie; Séguard, Céline; Couraud, Pierre-Olivier; Weksler, Babette B; Petry, Klaus G; Gaudin, Karen

    2015-04-15

    A Reversed Phase-High Performance Liquid Chromatography/Diode Array Detection method was developed and validated for paracetamol quantification in cell culture fluid from an in vitro Blood Brain Barrier model. The chromatographic method and sample preparation were developed using only aqueous solvents. The column was a XTerra RP18 150 × 4.6mm, 3.5 μm with a guard column XTerra RP18 20 × 4.6 mm, 3.5 μm at 35 °C and the mobile phase was composed by 100% formate buffer 20 mM at pH 4 and flow rate was set at 1 mL/min. The detection was at 242 nm. The sample was injected at 10 μL. Validation was performed using the accuracy profile approach. The analytical procedure was validated with the acceptance limits at ± 10% over a range of concentration from 1 to 58 mg L(-1). The procedure was then used in routine to determine paracetamol concentration in a brain blood barrier in vitro model. Application of the Unither paracetamol formulation in Blood Brain Barrier model allowed the determination and comparison of the transcellular passage of paracetamol at 37 °C and 4 °C, that excludes paracellular or non specific leakage.

  11. Validating An Analytic Completeness Model for Kepler Target Stars Based on Flux-level Transit Injection Experiments

    Science.gov (United States)

    Catanzarite, Joseph; Burke, Christopher J.; Li, Jie; Seader, Shawn; Haas, Michael R.; Batalha, Natalie; Henze, Christopher; Christiansen, Jessie; Kepler Project, NASA Advanced Supercomputing Division

    2016-06-01

    The Kepler Mission is developing an Analytic Completeness Model (ACM) to estimate detection completeness contours as a function of exoplanet radius and period for each target star. Accurate completeness contours are necessary for robust estimation of exoplanet occurrence rates.The main components of the ACM for a target star are: detection efficiency as a function of SNR, the window function (WF) and the one-sigma depth function (OSDF). (Ref. Burke et al. 2015). The WF captures the falloff in transit detection probability at long periods that is determined by the observation window (the duration over which the target star has been observed). The OSDF is the transit depth (in parts per million) that yields SNR of unity for the full transit train. It is a function of period, and accounts for the time-varying properties of the noise and for missing or deweighted data.We are performing flux-level transit injection (FLTI) experiments on selected Kepler target stars with the goal of refining and validating the ACM. “Flux-level” injection machinery inserts exoplanet transit signatures directly into the flux time series, as opposed to “pixel-level” injection, which inserts transit signatures into the individual pixels using the pixel response function. See Jie Li's poster: ID #2493668, "Flux-level transit injection experiments with the NASA Pleiades Supercomputer" for details, including performance statistics.Since FLTI is affordable for only a small subset of the Kepler targets, the ACM is designed to apply to most Kepler target stars. We validate this model using “deep” FLTI experiments, with ~500,000 injection realizations on each of a small number of targets and “shallow” FLTI experiments with ~2000 injection realizations on each of many targets. From the results of these experiments, we identify anomalous targets, model their behavior and refine the ACM accordingly.In this presentation, we discuss progress in validating and refining the ACM, and we

  12. Application of Analytical Quality by Design concept for bilastine and its degradation impurities determination by hydrophilic interaction liquid chromatographic method.

    Science.gov (United States)

    Terzić, Jelena; Popović, Igor; Stajić, Ana; Tumpa, Anja; Jančić-Stojanović, Biljana

    2016-06-05

    This paper deals with the development of hydrophilic interaction liquid chromatographic (HILIC) method for the analysis of bilastine and its degradation impurities following Analytical Quality by Design approach. It is the first time that the method for bilastine and its impurities is proposed. The main objective was to identify the conditions where an adequate separation in minimal analysis duration could be achieved within a robust region. Critical process parameters which have the most influence on method performance were defined as acetonitrile content in the mobile phase, pH of the aqueous phase and ammonium acetate concentration in the aqueous phase. Box-Behnken design was applied for establishing a relationship between critical process parameters and critical quality attributes. The defined mathematical models and Monte Carlo simulations were used to identify the design space. Fractional factorial design was applied for experimental robustness testing and the method is validated to verify the adequacy of selected optimal conditions: the analytical column Luna(®) HILIC (100mm×4.6mm, 5μm particle size); mobile phase consisted of acetonitrile-aqueous phase (50mM ammonium acetate, pH adjusted to 5.3 with glacial acetic acid) (90.5:9.5, v/v); column temperature 30°C, mobile phase flow rate 1mLmin(-1), wavelength of detection 275nm.

  13. Possibilities of Utilizing the Method of Analytical Hierarchy Process Within the Strategy of Corporate Social Business

    Science.gov (United States)

    Drieniková, Katarína; Hrdinová, Gabriela; Naňo, Tomáš; Sakál, Peter

    2010-01-01

    The paper deals with the analysis of the theory of corporate social responsibility, risk management and the exact method of analytic hierarchic process that is used in the decision-making processes. The Chapters 2 and 3 focus on presentation of the experience with the application of the method in formulating the stakeholders' strategic goals within the Corporate Social Responsibility (CSR) and simultaneously its utilization in minimizing the environmental risks. The major benefit of this paper is the application of Analytical Hierarchy Process (AHP).

  14. 2D Stabilised analytic signal method in DC pole-pole potential data interpretation

    Indian Academy of Sciences (India)

    Paras R Pujari; Rambhatla G Sastry

    2003-03-01

    Using analytic signal method, interpretation of pole-pole secondary electric potentials due to 2D conductive/resistive prisms is presented. The estimated parameters are the location, lateral extent or width and depth to top surface of the prism. Forward modelling is attempted by 2D-Finite Difference method. The proposed stabilised analytic signal algorithm (RES2AS) uses Tikhonov's regularization scheme and FFT routines. The algorithm is tested on three theoretical examples and field data from the campus of Roorkee University. The stability of RES2AS is also tested on synthetic error prone secondary pole-pole potential data.

  15. Study of Injection Molding Warpage Using Analytic Hierarchy Process and Taguchi Method

    Directory of Open Access Journals (Sweden)

    Dyi-Cheng Chen

    2016-10-01

    Full Text Available This study integrated Analytic Hierarchy Process and Taguchi method to investigate into injection molding warpage. The warpage important factor will be elected by Analytic Hierarchy Process (AHP, the AHP hierarchy analysis factor from documents collected and aggregate out data, then through the expert questionnaire delete low weight factor. Finally, we used Taguchi quality engineering method to decide injection molding optimized combination factors. Furthermore, the paper used injection pressure, holding pressure, holding time, mold temperature to analyze four factors, three levels Taguchi design data. Moreover, the paper discussed the reaction of each factor on the S / N ratio and analysis of variance to obtain the best combination of minimal warpage.

  16. Aspects of investigating scrambling in the synthesis of porphyrins Different analytical methods

    DEFF Research Database (Denmark)

    Nielsen, C.B.; Krebs, Frederik C

    2005-01-01

    Herein, we discuss the analyses and quantification of the different components in porphyrin mixtures, prepared from p-anisaidehyde, p-tolualdehyde, and 5-(4-bromophenyl)-dipyrromethane with acid catalysis, using NMR and HPLC. The advantages and disadvantages of these analytical methods are emphas......Herein, we discuss the analyses and quantification of the different components in porphyrin mixtures, prepared from p-anisaidehyde, p-tolualdehyde, and 5-(4-bromophenyl)-dipyrromethane with acid catalysis, using NMR and HPLC. The advantages and disadvantages of these analytical methods...

  17. A new validated method for the simultaneous determination of benzocaine, propylparaben and benzyl alcohol in a bioadhesive gel by HPLC.

    Science.gov (United States)

    Pérez-Lozano, P; García-Montoya, E; Orriols, A; Miñarro, M; Ticó, J R; Suñé-Negre, J M

    2005-10-04

    A new HPLC-RP method has been developed and validated for the simultaneous determination of benzocaine, two preservatives (propylparaben (nipasol) and benzyl alcohol) and degradation products of benzocaine in a semisolid pharmaceutical dosage form (benzocaine gel). The method uses a Nucleosil 120 C18 column and gradient elution. The mobile phase consisted of a mixture of methanol and glacial acetic acid (10%, v/v) at different proportion according to a time-schedule programme, pumped at a flow rate of 2.0 ml min(-1). The DAD detector was set at 258 nm. The validation study was carried out fulfilling the ICH guidelines in order to prove that the new analytical method, meets the reliability characteristics, and these characteristics showed the capacity of analytical method to keep, throughout the time, the fundamental criteria for validation: selectivity, linearity, precision, accuracy and sensitivity. The method was applied during the quality control of benzocaine gel in order to quantify the drug (benzocaine), preservatives and degraded products and proved to be suitable for rapid and reliable quality control method.

  18. Quantitative bioanalytical and analytical method development of dibenzazepine derivative, carbamazepine: A review

    OpenAIRE

    Prasanna A. Datar

    2015-01-01

    Bioanalytical methods are widely used for quantitative estimation of drugs and their metabolites in physiological matrices. These methods could be applied to studies in areas of human clinical pharmacology and toxicology. The major bioanalytical services are method development, method validation and sample analysis (method application). Various methods such as GC, LC–MS/MS, HPLC, HPTLC, micellar electrokinetic chromatography, and UFLC have been used in laboratories for the qualitative and qua...

  19. Development and validation of an extraction method for the analysis of perfluoroalkyl substances in human hair.

    Science.gov (United States)

    Kim, Da-Hye; Oh, Jeong-Eun

    2017-02-16

    Human hair has many advantages as a non-invasive sample; however, analytical methods for detecting perfluoroalkyl substances (PFASs) in human hair are still in the development stage. Therefore, the aim of this study was to develop and validate a method for monitoring 11 PFASs in human hair. Solid-phase extraction (SPE), ion-pairing extraction (IPE), a combined method (SPE+IPE) and solvent extraction with ENVI-carb clean-up were compared to develop an optimal extraction method using two types of hair sample (powder and piece forms). Analysis of PFASs was performed using liquid chromatography and tandem mass spectrometry. Among the four different extraction procedures, the SPE method using powdered hair showed the best extraction efficiency and recoveries ranged from 85.8 to 102%. The method detection limits for the SPE method were 0.114-0.796 ng/g and good precision (below 10%) and accuracy (66.4-110%) were obtained. In light of these results, SPE is considered the optimal method for PFAS extraction from hair. It was also successfully used to detect PFASs in human hair samples.

  20. Guidance for characterizing explosives contaminated soils: Sampling and selecting on-site analytical methods

    Energy Technology Data Exchange (ETDEWEB)

    Crockett, A.B. [Idaho National Engineering Lab., Idaho Falls, ID (United States); Craig, H.D. [Environmental Protection Agency, Portland, OR (United States). Oregon Operations Office; Jenkins, T.F. [Army Cold Regions Research and Engineering Lab., Hanover, NH (United States); Sisk, W.E. [Army Environmental Center, Aberdeen Proving Grounds, MD (United States)

    1996-09-01

    A large number of defense-related sites are contaminated with elevated levels of secondary explosives. Levels of contamination range from barely detectable to levels above 10% that need special handling due to the detonation potential. Characterization of explosives-contaminated sites is particularly difficult due to the very heterogeneous distribution of contamination in the environment and within samples. To improve site characterization, several options exist including collecting more samples, providing on-site analytical data to help direct the investigation, compositing samples, improving homogenization of samples, and extracting larger samples. On-site analytical methods are essential to more economical and improved characterization. On-site methods might suffer in terms of precision and accuracy, but this is more than offset by the increased number of samples that can be run. While verification using a standard analytical procedure should be part of any quality assurance program, reducing the number of samples analyzed by the more expensive methods can result in significantly reduced costs. Often 70 to 90% of the soil samples analyzed during an explosives site investigation do not contain detectable levels of contamination. Two basic types of on-site analytical methods are in wide use for explosives in soil, calorimetric and immunoassay. Calorimetric methods generally detect broad classes of compounds such as nitroaromatics or nitramines, while immunoassay methods are more compound specific. Since TNT or RDX is usually present in explosive-contaminated soils, the use of procedures designed to detect only these or similar compounds can be very effective.