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Sample records for clot method validation

  1. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation

    International Nuclear Information System (INIS)

    Fukumori, Neuza Taeko Okasaki

    2008-01-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the 131 I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL -1 (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL -1 , to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products 131 I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get valuable quantitative and

  2. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation; Determinacao de endotoxina bacteriana (pirogenio) em radiofarmacos pelo metodo de formacao de gel. Validacao

    Energy Technology Data Exchange (ETDEWEB)

    Fukumori, Neuza Taeko Okasaki

    2008-07-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the {sup 131}I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL{sup -1} (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL{sup -1}, to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products {sup 131}I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get valuable

  3. Determination of bacterial endotoxin (pyrogen) in radiopharmaceuticals by the gel clot method. Validation; Determinacao de endotoxina bacteriana (pirogenio) em radiofarmacos pelo metodo de formacao de gel. Validacao

    Energy Technology Data Exchange (ETDEWEB)

    Fukumori, Neuza Taeko Okasaki

    2008-07-01

    Before the Limulus amebocyte lysate (LAL) test, the only available means of pirogenicity testing for parenteral drugs and medical devices was the United States Pharmacopoeia (USP) rabbit pyrogen test. Especially for radiopharmaceuticals, the LAL assay is the elective way to determine bacterial endotoxin. The aim of this work was to validate the gel clot method for some radiopharmaceuticals without measurable interference. The FDA's LALTest guideline defines interference as a condition that causes a significant difference between the endpoints of a positive water control and positive product control series using a standard endotoxin. Experiments were performed in accordance to the USP bacterial endotoxins test in the {sup 131}I- m-iodobenzylguanidine; the radioisotopes Gallium-67 and Thallium-201; the lyophilized reagents DTPA, Phytate, GHA, HSA and Colloidal Tin. The Maximum Valid Dilution (MVD) was calculated for each product based upon the clinical dose of the material and a twofold serial dilution below the MVD was performed in duplicate to detect interferences. The labeled sensitivity of the used LAL reagent was 0.125 EU mL{sup -1} (Endotoxin Units per milliliter). For validation, a dilution series was performed, a twofold dilution of control standard endotoxin (CSE) from 0.5 to 0.03 EU mL{sup -1}, to confirm the labeled sensitivity of the LAL reagent being tested in sterile and non pyrogenic water, in quadruplicate. The same dilution series was performed with the CSE and the product in the 1:100 dilution factor, in three consecutive batches of each radiopharmaceutical. The products {sup 131}I-m-iodobenzylguanidine, Gallium-67, Thallium-201, DTPA, HSA and Colloidal Tin were found compatible with the LAL test at a 1:100 dilution factor. Phytate and GHA showed some interference in the gel clot test. Other techniques to determine endotoxins as the chromogenic (color development) and the turbidimetric test (turbidity development), were also assessed to get

  4. Platelet Counts in Insoluble Platelet-Rich Fibrin Clots: A Direct Method for Accurate Determination

    Directory of Open Access Journals (Sweden)

    Yutaka Kitamura

    2018-02-01

    Full Text Available Platelet-rich fibrin (PRF clots have been used in regenerative dentistry most often, with the assumption that growth factor levels are concentrated in proportion to the platelet concentration. Platelet counts in PRF are generally determined indirectly by platelet counting in other liquid fractions. This study shows a method for direct estimation of platelet counts in PRF. To validate this method by determination of the recovery rate, whole-blood samples were obtained with an anticoagulant from healthy donors, and platelet-rich plasma (PRP fractions were clotted with CaCl2 by centrifugation and digested with tissue-plasminogen activator. Platelet counts were estimated before clotting and after digestion using an automatic hemocytometer. The method was then tested on PRF clots. The quality of platelets was examined by scanning electron microscopy and flow cytometry. In PRP-derived fibrin matrices, the recovery rate of platelets and white blood cells was 91.6 and 74.6%, respectively, after 24 h of digestion. In PRF clots associated with small and large red thrombi, platelet counts were 92.6 and 67.2% of the respective total platelet counts. These findings suggest that our direct method is sufficient for estimating the number of platelets trapped in an insoluble fibrin matrix and for determining that platelets are distributed in PRF clots and red thrombi roughly in proportion to their individual volumes. Therefore, we propose this direct digestion method for more accurate estimation of platelet counts in most types of platelet-enriched fibrin matrix.

  5. Building and validation of a prognostic model for predicting extracorporeal circuit clotting in patients with continuous renal replacement therapy.

    Science.gov (United States)

    Fu, Xia; Liang, Xinling; Song, Li; Huang, Huigen; Wang, Jing; Chen, Yuanhan; Zhang, Li; Quan, Zilin; Shi, Wei

    2014-04-01

    To develop a predictive model for circuit clotting in patients with continuous renal replacement therapy (CRRT). A total of 425 cases were selected. 302 cases were used to develop a predictive model of extracorporeal circuit life span during CRRT without citrate anticoagulation in 24 h, and 123 cases were used to validate the model. The prediction formula was developed using multivariate Cox proportional-hazards regression analysis, from which a risk score was assigned. The mean survival time of the circuit was 15.0 ± 1.3 h, and the rate of circuit clotting was 66.6 % during 24 h of CRRT. Five significant variables were assigned a predicting score according to the regression coefficient: insufficient blood flow, no anticoagulation, hematocrit ≥0.37, lactic acid of arterial blood gas analysis ≤3 mmol/L and APTT R (2) = 0.232; P = 0.301). A risk score that includes the five above-mentioned variables can be used to predict the likelihood of extracorporeal circuit clotting in patients undergoing CRRT.

  6. Blood Clots

    Science.gov (United States)

    ... sitting for long periods. If you travel by airplane, walk the aisle periodically. For long car trips, ... Your-Risk-for-Excessive-Blood-Clotting_UCM_448771_Article.jsp. Accessed April 18, 2016. What causes excessive ...

  7. Blood Clots

    Science.gov (United States)

    ... Pregnancy Immobility (including prolonged inactivity, long trips by plane or car ) Smoking Oral contraceptives Certain cancers Trauma Certain surgeries Age (increased risk for people over age 60) A family history of blood clots Chronic inflammatory diseases Diabetes High ...

  8. Comparison of standard fibrinogen measurement methods with fibrin clot firmness assessed by thromboelastometry in patients with cirrhosis.

    Science.gov (United States)

    Vucelic, Dragica; Jesic, Rada; Jovicic, Snezana; Zivotic, Maja; Grubor, Nikica; Trajkovic, Goran; Canic, Ivana; Elezovic, Ivo; Antovic, Aleksandra

    2015-06-01

    The Clauss fibrinogen method and thrombin clotting time (TCT) are still routinely used in patients with cirrhosis to define fibrinogen concentration and clotting potential. The thromboelastometric functional fibrinogen FIBTEM assay evaluates the strength of fibrin-based clots in whole blood, providing information on both quantitative deficit and fibrin polymerization disorders. To compare these three methods of assessing fibrinogen in patients with cirrhosis of different aetiologies, characterized by impairment in fibrinogen concentration as well as functional aberrance. Sixty patients with alcoholic and 24 patients with cholestatic cirrhosis were included (Child-Pugh score (CPs)A, n=24; B, n=32; C, n=28). All parameters were compared with those from a control group. Maximum clot firmness (MCF) in the FIBTEM test was assessed in regard to its relevance in detection of qualitative fibrinogen disorders in comparison with results obtained by standard measurement methods, i.e. the Clauss fibrinogen method and TCT. With increased cirrhosis severity, fibrinogen and FIBTEM-MCF levels significantly declined (p=0.002), while TCT was significantly prolonged (p=0.002). In all CPs groups, fibrinogen strongly correlated with FIBTEM-MCF (r=0.77, r=0.72, r=0.74; pmeasurement in cirrhotic patients, especially in evaluating fibrin polymerization disorders in these patients. Further studies are needed to evaluate the usefulness of this assay in predicting bleeding complications in cirrhotic patients as well as monitoring replacement treatment. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... For Patients Blood Disorders Blood Clots Blood Clotting & Pregnancy If you are pregnant, or you have just ... The risk of developing a blood clot during pregnancy is increased by the following: Previous blood clots ...

  10. Blood Clotting and Pregnancy

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    Full Text Available ... Blood Basics Blood Disorders Anemia Bleeding Disorders Blood Cancers Blood Clots Blood Clotting and Pregnancy Clots and ... Increased maternal age Other medical illness (e.g., cancer, infection) back to top How are Blood Clots ...

  11. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... of articles from the 2017 ASH Annual Meeting Education Program Blood: How I Treat A compendium of Blood articles updated ... Clots Blood Clotting and Pregnancy Clots and Travel DVT Myths vs. Facts Blood ...

  12. Blood Clotting and Pregnancy

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    Full Text Available ... Blood Clots Blood Clotting and Pregnancy Clots and Travel DVT Myths vs. Facts Blood Disorder Fact Sheets ... that occurs when a DVT breaks off and travels to the blood vessels of the lungs. DVT ...

  13. Blood Clotting and Pregnancy

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    Full Text Available ... back to top How are Blood Clots in Pregnant Women Treated? Typically, blood clots are treated with ... you think you have one. If you are pregnant and have concerns about blood clots, talk with ...

  14. Blood Clotting and Pregnancy

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    Full Text Available ... Section Action Alerts Advocacy Toolkit Policy News Sickle Cell Disease Initiative Policy Statements Congressional Fellowship Testimony and ... Blood Basics Blood Disorders Anemia Bleeding Disorders Blood Cancers Blood Clots Blood Clotting and Pregnancy Clots and ...

  15. Blood Clotting and Pregnancy

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    Full Text Available ... blood clots are treated with an anticoagulant, a medicine that prevents the blood from clotting. Certain anticoagulants are safe to use during pregnancy. back to top Are Blood Clots Preventable? There ...

  16. Blood Clotting and Pregnancy

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    Full Text Available ... clot. Blood clots in pregnant women tend to form in the deep veins of the legs or ... potentially dangerous to your baby. Blood clots can form inside the placenta, cutting off blood flow and ...

  17. Blood Clotting and Pregnancy

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    Full Text Available ... resource to help stay current with the latest advances in the field Hematology 2017 A collection of articles ... Disorders Blood Cancers Blood Clots Blood Clotting and Pregnancy Clots and ...

  18. Blood Clotting and Pregnancy

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    Full Text Available ... all publications For Patients Blood Basics Blood Disorders Anemia Bleeding Disorders Blood Cancers Blood Clots Blood Clotting and Pregnancy Clots and Travel DVT Myths vs. Facts Blood ...

  19. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... with Your Doctor Patient Group Links Advocacy Toolkit Home For Patients Blood Disorders Blood Clots Blood Clotting & Pregnancy If you are pregnant, or you have just had a baby, you are at greater risk of developing a blood clot. Blood clots in pregnant women tend to form in the deep veins of ...

  20. Blood Clotting and Pregnancy

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    Full Text Available ... these blood conditions and increase research on the causes, prevention, and treatment. Blood clots are also potentially ... Increased maternal age Other medical illness (e.g., cancer, infection) back to top How are Blood Clots ...

  1. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... increased by the following: Previous blood clots A genetic predisposition to blood clots Obesity Prolonged immobility (e. ... Be aware of risk factors. Know your family history. Make sure your doctor knows about any history ...

  2. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... Be aware of risk factors. Know your family history. Make sure your doctor knows about any history of blood clots or blood clotting disorders in ... Support Opportunities | Privacy Policy | Terms of Service | Contact Us

  3. Blood Clotting and Pregnancy

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    Full Text Available ... In This Section Agenda for Hematology Research Precision Medicine Initiative Research Registry Research Recommendations Research Programs and ... blood clots are treated with an anticoagulant, a medicine that prevents the blood from clotting. Certain anticoagulants ...

  4. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... pregnancy: Be aware of risk factors. Know your family history. Make sure your doctor knows about any ... blood clots or blood clotting disorders in your family. Remain active, with your doctor's approval. Be aware ...

  5. Blood Clotting and Pregnancy

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    Full Text Available ... harming your baby. Jump To: Am I at Risk? The risk of developing a blood clot during pregnancy is ... prevent blood clots during pregnancy: Be aware of risk factors. Know your family history. Make sure your ...

  6. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... are pregnant, or you have just had a baby, you are at greater risk of developing a ... Blood clots are also potentially dangerous to your baby. Blood clots can form inside the placenta, cutting ...

  7. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... to top How are Blood Clots in Pregnant Women Treated? Typically, blood clots are treated with an ... 0544 | Fax 202-776-0545 ASH Store ASH Job Center ASH Apps Share Your Idea Donate Research ...

  8. Blood Clotting and Pregnancy

    Science.gov (United States)

    ... blood clots A genetic predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) Multiple births Increased maternal age Other medical illness (e.g., cancer, infection) ...

  9. Blood Clotting and Pregnancy

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    Full Text Available ... blood clots A genetic predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) Multiple births Increased maternal age Other medical illness (e.g., cancer, infection) ...

  10. Blood Clotting and Pregnancy

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    Full Text Available ... an immediate impact on your practice Summit on Emerging Immunotherapies Registration Schedule & Program Meeting on Lymphoma Biology ... blood clots are treated with an anticoagulant, a medicine that prevents the blood from clotting. Certain anticoagulants ...

  11. Blood Clotting and Pregnancy

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    Full Text Available ... increased by the following: Previous blood clots A genetic predisposition to blood clots Obesity Prolonged immobility (e. ... 2018 by American Society of Hematology Support Opportunities | Privacy Policy | Terms of Service | Contact Us

  12. Blood Clotting and Pregnancy

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    Full Text Available ... blood clots A genetic predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) ... of practicing hematologists in your area. Learn more AMERICAN SOCIETY OF HEMATOLOGY 2021 L Street NW, Suite ...

  13. Blood Clotting and Pregnancy

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    Full Text Available ... to top How are Blood Clots in Pregnant Women Treated? Typically, blood clots are treated with an ... Image Bank Advocacy Action Alerts Policy News Advocacy Leadership Institute Policy Statements Testimony & Correspondence Meetings ASH Annual ...

  14. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... presentations, that can help you make an immediate impact on your practice Summit on Emerging Immunotherapies Registration ... blood clots are treated with an anticoagulant, a medicine that prevents the blood from clotting. Certain anticoagulants ...

  15. Blood Clotting and Pregnancy

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    Full Text Available ... to top How are Blood Clots in Pregnant Women Treated? Typically, blood clots are treated with an ... of Web links to patient groups and other organizations that provide information. back to top ASH Foundation ...

  16. Blood Clotting and Pregnancy

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    Full Text Available ... This Section Action Alerts Advocacy Toolkit Policy News Sickle Cell Disease Initiative Policy Statements Congressional Fellowship Testimony and ... all publications For Patients Blood Basics Blood Disorders Anemia Bleeding Disorders Blood Cancers Blood Clots Blood Clotting ...

  17. Blood Clotting and Pregnancy

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    Full Text Available ... to top How are Blood Clots in Pregnant Women Treated? Typically, blood clots are treated with an ... Programs and Awards ASH Agenda for Hematology Research Education For Clinicians For Trainees For Educators For Patients ...

  18. Validation Process Methods

    Energy Technology Data Exchange (ETDEWEB)

    Lewis, John E. [National Renewable Energy Lab. (NREL), Golden, CO (United States); English, Christine M. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Gesick, Joshua C. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Mukkamala, Saikrishna [National Renewable Energy Lab. (NREL), Golden, CO (United States)

    2018-01-04

    This report documents the validation process as applied to projects awarded through Funding Opportunity Announcements (FOAs) within the U.S. Department of Energy Bioenergy Technologies Office (DOE-BETO). It describes the procedures used to protect and verify project data, as well as the systematic framework used to evaluate and track performance metrics throughout the life of the project. This report also describes the procedures used to validate the proposed process design, cost data, analysis methodologies, and supporting documentation provided by the recipients.

  19. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... known as venous thromboembolism, are highly preventable (see prevention tips below). The U.S. Surgeon General has issued ... blood conditions and increase research on the causes, prevention, and treatment. Blood clots are also potentially dangerous ...

  20. Blood Clotting and Pregnancy

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    Full Text Available ... predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) Multiple births Increased maternal age Other medical illness (e.g., cancer, infection) back to top How are Blood ...

  1. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... to help stay current with the latest advances in the field Hematology 2017 A collection of articles from ... Blood clots in pregnant women tend to form in the deep veins of the legs or in the ...

  2. Postpartum Blood Clots

    Science.gov (United States)

    ... Video) Fetal Ultrasound Scanning Additional Content Medical News Postpartum Blood Clots By Julie S. Moldenhauer, MD, Associate Professor ... Professional Version Postdelivery Period Overview of the Postdelivery (Postpartum) Period Postpartum Infections Postpartum Infections of the Uterus ...

  3. Blood Clotting and Pregnancy

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    Full Text Available ... Action on DVT and PE to raise public awareness of these blood conditions and increase research on ... Increased maternal age Other medical illness (e.g., cancer, infection) back to top How are Blood Clots ...

  4. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... of articles from the 2017 ASH Annual Meeting Education Program Blood: How I Treat A compendium of Blood articles ... Pregnancy Clots and Travel DVT Myths vs. Facts Blood Disorder Fact Sheets ...

  5. Blood Clotting and Pregnancy

    Medline Plus

    Full Text Available ... genetic predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) Multiple births Increased maternal age Other medical illness (e.g., cancer, infection) back to top How are ...

  6. Blood Clotting and Pregnancy

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    Full Text Available ... A genetic predisposition to blood clots Obesity Prolonged immobility (e.g., bedrest, long distance travel) Multiple births ... treating blood conditions. back to top Antiphospholipid Antibody Syndrome: A Patient's Journey back to top Where Can ...

  7. Blood Clotting and Pregnancy

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    Full Text Available ... harming your baby. Jump To: Am I at Risk? The risk of developing a blood clot during ... Advances The Hematologist ASH Clinical News ASH Self-Assessment Program Hematology , ASH Education Program About Awards Membership ...

  8. Blood Clotting and Pregnancy

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    Full Text Available ... have one. If you are pregnant and have concerns about blood clots, talk with your doctor about ... 2018 by American Society of Hematology Support Opportunities | Privacy Policy | Terms of Service | Contact Us

  9. Blood Clotting and Pregnancy

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    Full Text Available ... are pregnant and have concerns about blood clots, talk with your doctor about your risks and prevention. Depending on your condition, your OB-GYN may refer you to a hematologist, a doctor who specializes in treating blood conditions. back to top ...

  10. Clot lysis time in platelet-rich plasma: method assessment, comparison with assays in platelet-free and platelet-poor plasmas, and response to tranexamic acid.

    Science.gov (United States)

    Panes, Olga; Padilla, Oslando; Matus, Valeria; Sáez, Claudia G; Berkovits, Alejandro; Pereira, Jaime; Mezzano, Diego

    2012-01-01

    Fibrinolysis dysfunctions cause bleeding or predisposition to thrombosis. Platelets contain several factors of the fibrinolytic system, which could up or down regulate this process. However, the temporal relationship and relative contributions of plasma and platelet components in clot lysis are mostly unknown. We developed a clot lysis time (CLT) assay in platelet-rich plasma (PRP-CLT, with and without stimulation) and compared it to a similar one in platelet-free plasma (PFP) and to another previously reported test in platelet-poor plasma (PPP). We also studied the differential effects of a single dose of tranexamic acid (TXA) on these tests in healthy subjects. PFP- and PPP-CLT were significantly shorter than PRP-CLT, and the three assays were highly correlated (p plasma PAI-1, von Willebrand factor, fibrinogen, LDL-cholesterol, and triglycerides (p platelet aggregation/secretion, platelet counts, and pro-coagulant tests to explore factor X activation by platelets, PRP clotting time, and thrombin generation in PRP. Among all the studied variables, PFP-CLT was independently associated with plasma PAI-1, LDL-cholesterol, and triglycerides and, additionally, stimulated PRP-CLT was also independently associated with plasma fibrinogen. A single 1 g dose of TXA strikingly prolonged all three CLTs, but in contrast to the results without the drug, the lysis times were substantially shorter in non-stimulated or stimulated PRP than in PFP and PPP. This standardized PRP-CLT may become a useful tool to study the role of platelets in clot resistance and lysis. Our results suggest that initially, the platelets enmeshed in the clot slow down the fibrinolysis process. However, the increased clot resistance to lysis induced by TXA is overcome earlier in platelet-rich clots than in PFP or PPP clots. This is likely explained by the display of platelet pro-fibrinolytic effects. Focused research is needed to disclose the mechanisms for the relationship between CLT and plasma

  11. Validation for chromatographic and electrophoretic methods

    OpenAIRE

    Ribani, Marcelo; Bottoli, Carla Beatriz Grespan; Collins, Carol H.; Jardim, Isabel Cristina Sales Fontes; Melo, Lúcio Flávio Costa

    2004-01-01

    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 dif...

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

    KAUST Repository

    Stripling, H.F.; Adams, M.L.; McClarren, R.G.; Mallick, B.K.

    2011-01-01

    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

  13. 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)

  14. Validated modified Lycopodium spore method development for ...

    African Journals Online (AJOL)

    Validated modified lycopodium spore method has been developed for simple and rapid quantification of herbal powdered drugs. Lycopodium spore method was performed on ingredients of Shatavaryadi churna, an ayurvedic formulation used as immunomodulator, galactagogue, aphrodisiac and rejuvenator. Estimation of ...

  15. Method Validation Procedure in Gamma Spectroscopy Laboratory

    International Nuclear Information System (INIS)

    El Samad, O.; Baydoun, R.

    2008-01-01

    The present work describes the methodology followed for the application of ISO 17025 standards in gamma spectroscopy laboratory at the Lebanese Atomic Energy Commission including the management and technical requirements. A set of documents, written procedures and records were prepared to achieve the management part. The technical requirements, internal method validation was applied through the estimation of trueness, repeatability , minimum detectable activity and combined uncertainty, participation in IAEA proficiency tests assure the external method validation, specially that the gamma spectroscopy lab is a member of ALMERA network (Analytical Laboratories for the Measurements of Environmental Radioactivity). Some of these results are presented in this paper. (author)

  16. Moving beyond Traditional Methods of Survey Validation

    Science.gov (United States)

    Maul, Andrew

    2017-01-01

    In his focus article, "Rethinking Traditional Methods of Survey Validation," published in this issue of "Measurement: Interdisciplinary Research and Perspectives," Andrew Maul wrote that it is commonly believed that self-report, survey-based instruments can be used to measure a wide range of psychological attributes, such as…

  17. Endogenous fibrinolysis facilitates clot retraction in vivo.

    Science.gov (United States)

    Samson, Andre L; Alwis, Imala; Maclean, Jessica A A; Priyananda, Pramith; Hawkett, Brian; Schoenwaelder, Simone M; Jackson, Shaun P

    2017-12-07

    Clot retraction refers to the process whereby activated platelets transduce contractile forces onto the fibrin network of a thrombus, which over time increases clot density and decreases clot size. This process is considered important for promoting clot stability and maintaining blood vessel patency. Insights into the mechanisms regulating clot retraction at sites of vascular injury have been hampered by a paucity of in vivo experimental models. By pairing localized vascular injury with thrombin microinjection in the mesenteric circulation of mice, we have demonstrated that the fibrin network of thrombi progressively compacts over a 2-hour period. This was a genuine retraction process, as treating thrombi with blebbistatin to inhibit myosin IIa-mediated platelet contractility prevented shrinkage of the fibrin network. Real-time confocal analysis of fibrinolysis after recombinant tissue-type plasminogen activator (tPA) administration revealed that incomplete proteolysis of fibrin polymers markedly facilitated clot retraction. Similarly, inhibiting endogenous fibrinolysis with tranexamic acid reduced retraction of fibrin polymers in vivo. In vitro clot retraction experiments indicated that subthreshold doses of tPA facilitated clot retraction through a plasmin-dependent mechanism. These effects correlated with changes in the elastic modulus of fibrin clots. These findings define the endogenous fibrinolytic system as an important regulator of clot retraction, and show that promoting clot retraction is a novel and complementary means by which fibrinolytic enzymes can reduce thrombus size. © 2017 by The American Society of Hematology.

  18. Thermal Blood Clot Formation and use in Microfluidic Device Valving Applications

    Science.gov (United States)

    Tai, Yu-Chong (Inventor); Shi, Wendian (Inventor); Guo, Luke (Inventor)

    2014-01-01

    The present invention provides a method of forming a blood-clot microvalve by heating blood in a capillary tube of a microfluidic device. Also described are methods of modulating liquid flow in a capillary tube by forming and removing a blood-clot microvalve.

  19. Estimativa da incerteza em ensaio de detecção de endotoxina bacteriana pelo método de gelificação Estimation of uncertainty in the detection of bacterial endotoxin by gel-clot method

    Directory of Open Access Journals (Sweden)

    Felipe Rebello Lourenço

    2005-12-01

    Full Text Available Desde a publicação da ISO 17025:1999, o interesse em métodos para estimativa da incerteza em ensaios qualitativos, do tipo "passa/não passa", têm ganho grande importância. Uma forma de estimar e informar a incerteza deste tipo de ensaio é o uso das probabilidades de respostas-falsas, particularmente falsos-positivos e falsos-negativos, determinados a partir do teorema de Bayes. O objetivo deste artigo é estabelecer um método para a estimativa de incerteza em ensaios de detecção de endotoxina bacteriana pelo método in vitro Limulus Amebocyte Lysate (LAL. Considerando a confirmação da sensibilidade do LAL e a validação do teste, a probabilidade de uma resposta falsa corresponde à soma da probabilidade dos resultados falso-negativos e falso-positivos. A partir dos resultados obtidos foi verificado que a etapa da confirmação da sensibilidade do LAL contribui para a incerteza de forma mais significativa (67,6% que a etapa de validação do teste (32,4%. Através de um procedimento simples, descrito neste artigo, e de dados obtidos a partir da confirmação da sensibilidade do LAL e validação do teste para um produto em questão é possível obter uma estimativa de incerteza razoável para o ensaio de detecção de endotoxinas bacterianas pelo método de gelificação.Since the publication of ISO 17025:1999, the interest in methods for estimation of the uncertainty in qualitative analysis, such as 'pass/fail', have became more important. The usual form of estimating and informing the uncertainty in this kind of analysis is the use of false-response rates, particularly false-positive and false-negative, determinated from Bayes theorem. The aim of this paper is establish a method for estimation of the uncertainty in the detection of bacterial endotoxins by in vitro Limulus Amebocyte Lysate (LAL test. Considering the confirmation of LAL sensitivity and the validation of the test, the probability of a false-response corresponds to the

  20. Validation of the Rotation Ratios Method

    International Nuclear Information System (INIS)

    Foss, O.A.; Klaksvik, J.; Benum, P.; Anda, S.

    2007-01-01

    Background: The rotation ratios method describes rotations between pairs of sequential pelvic radiographs. The method seems promising but has not been validated. Purpose: To validate the accuracy of the rotation ratios method. Material and Methods: Known pelvic rotations between 165 radiographs obtained from five skeletal pelvises in an experimental material were compared with the corresponding calculated rotations to describe the accuracy of the method. The results from a clinical material of 262 pelvic radiographs from 46 patients defined the ranges of rotational differences compared. Repeated analyses, both on the experimental and the clinical material, were performed using the selected reference points to describe the robustness and the repeatability of the method. Results: The reference points were easy to identify and barely influenced by pelvic rotations. The mean differences between calculated and real pelvic rotations were 0.0 deg (SD 0.6) for vertical rotations and 0.1 deg (SD 0.7) for transversal rotations in the experimental material. The intra- and interobserver repeatability of the method was good. Conclusion: The accuracy of the method was reasonably high, and the method may prove to be clinically useful

  1. Model-Based Method for Sensor Validation

    Science.gov (United States)

    Vatan, Farrokh

    2012-01-01

    Fault detection, diagnosis, and prognosis are essential tasks in the operation of autonomous spacecraft, instruments, and in situ platforms. One of NASA s key mission requirements is robust state estimation. Sensing, using a wide range of sensors and sensor fusion approaches, plays a central role in robust state estimation, and there is a need to diagnose sensor failure as well as component failure. Sensor validation can be considered to be part of the larger effort of improving reliability and safety. The standard methods for solving the sensor validation problem are based on probabilistic analysis of the system, from which the method based on Bayesian networks is most popular. Therefore, these methods can only predict the most probable faulty sensors, which are subject to the initial probabilities defined for the failures. The method developed in this work is based on a model-based approach and provides the faulty sensors (if any), which can be logically inferred from the model of the system and the sensor readings (observations). The method is also more suitable for the systems when it is hard, or even impossible, to find the probability functions of the system. The method starts by a new mathematical description of the problem and develops a very efficient and systematic algorithm for its solution. The method builds on the concepts of analytical redundant relations (ARRs).

  2. Spacecraft early design validation using formal methods

    International Nuclear Information System (INIS)

    Bozzano, Marco; Cimatti, Alessandro; Katoen, Joost-Pieter; Katsaros, Panagiotis; Mokos, Konstantinos; Nguyen, Viet Yen; Noll, Thomas; Postma, Bart; Roveri, Marco

    2014-01-01

    The size and complexity of software in spacecraft is increasing exponentially, and this trend complicates its validation within the context of the overall spacecraft system. Current validation methods are labor-intensive as they rely on manual analysis, review and inspection. For future space missions, we developed – with challenging requirements from the European space industry – a novel modeling language and toolset for a (semi-)automated validation approach. Our modeling language is a dialect of AADL and enables engineers to express the system, the software, and their reliability aspects. The COMPASS toolset utilizes state-of-the-art model checking techniques, both qualitative and probabilistic, for the analysis of requirements related to functional correctness, safety, dependability and performance. Several pilot projects have been performed by industry, with two of them having focused on the system-level of a satellite platform in development. Our efforts resulted in a significant advancement of validating spacecraft designs from several perspectives, using a single integrated system model. The associated technology readiness level increased from level 1 (basic concepts and ideas) to early level 4 (laboratory-tested)

  3. Fluid Mechanics of Blood Clot Formation.

    Science.gov (United States)

    Fogelson, Aaron L; Neeves, Keith B

    2015-01-01

    Intravascular blood clots form in an environment in which hydrodynamic forces dominate and in which fluid-mediated transport is the primary means of moving material. The clotting system has evolved to exploit fluid dynamic mechanisms and to overcome fluid dynamic challenges to ensure that clots that preserve vascular integrity can form over the wide range of flow conditions found in the circulation. Fluid-mediated interactions between the many large deformable red blood cells and the few small rigid platelets lead to high platelet concentrations near vessel walls where platelets contribute to clotting. Receptor-ligand pairs with diverse kinetic and mechanical characteristics work synergistically to arrest rapidly flowing cells on an injured vessel. Variations in hydrodynamic stresses switch on and off the function of key clotting polymers. Protein transport to, from, and within a developing clot determines whether and how fast it grows. We review ongoing experimental and modeling research to understand these and related phenomena.

  4. Space Suit Joint Torque Measurement Method Validation

    Science.gov (United States)

    Valish, Dana; Eversley, Karina

    2012-01-01

    In 2009 and early 2010, a test method was developed and performed to quantify the torque required to manipulate joints in several existing operational and prototype space suits. This was done in an effort to develop joint torque requirements appropriate for a new Constellation Program space suit system. The same test method was levied on the Constellation space suit contractors to verify that their suit design met the requirements. However, because the original test was set up and conducted by a single test operator there was some question as to whether this method was repeatable enough to be considered a standard verification method for Constellation or other future development programs. In order to validate the method itself, a representative subset of the previous test was repeated, using the same information that would be available to space suit contractors, but set up and conducted by someone not familiar with the previous test. The resultant data was compared using graphical and statistical analysis; the results indicated a significant variance in values reported for a subset of the re-tested joints. Potential variables that could have affected the data were identified and a third round of testing was conducted in an attempt to eliminate and/or quantify the effects of these variables. The results of the third test effort will be used to determine whether or not the proposed joint torque methodology can be applied to future space suit development contracts.

  5. Comparison of validation methods for forming simulations

    Science.gov (United States)

    Schug, Alexander; Kapphan, Gabriel; Bardl, Georg; Hinterhölzl, Roland; Drechsler, Klaus

    2018-05-01

    The forming simulation of fibre reinforced thermoplastics could reduce the development time and improve the forming results. But to take advantage of the full potential of the simulations it has to be ensured that the predictions for material behaviour are correct. For that reason, a thorough validation of the material model has to be conducted after characterising the material. Relevant aspects for the validation of the simulation are for example the outer contour, the occurrence of defects and the fibre paths. To measure these features various methods are available. Most relevant and also most difficult to measure are the emerging fibre orientations. For that reason, the focus of this study was on measuring this feature. The aim was to give an overview of the properties of different measuring systems and select the most promising systems for a comparison survey. Selected were an optical, an eddy current and a computer-assisted tomography system with the focus on measuring the fibre orientations. Different formed 3D parts made of unidirectional glass fibre and carbon fibre reinforced thermoplastics were measured. Advantages and disadvantages of the tested systems were revealed. Optical measurement systems are easy to use, but are limited to the surface plies. With an eddy current system also lower plies can be measured, but it is only suitable for carbon fibres. Using a computer-assisted tomography system all plies can be measured, but the system is limited to small parts and challenging to evaluate.

  6. Pro blood clotting activity of Scoparia dulcis in rats.

    Science.gov (United States)

    Ediriweera, E R H S S; Jayakody, J R A C; Ratnasooriya, W D

    2011-04-01

    Scoparia dulcis Linn (Family: Scrophulariaceae, Sinhala: WalKoththamalli) is a perennial herb growing in many tropical countries including Sri Lanka. Traditional Physicians in rural down south areas apply crushed S. dulcis plant on cuts and bruises to stop bleeding. S. dulcis may also have Rakta Sthambhana property. The study on effect of decoction (water extract) of S. dulcis on blood clotting time in rats was carried out to investigate this. Two groups of rats, 12 males and 42 females were used in this experimental study. Forty-two female rats were assigned into seven equal groups (n = 6/gp). Different doses of DE (25, 50, 100, 1000, 1500 mg/kg) (group 1-5) or 2 ml of distilled water (DW) (group 6) were orally administered. 0.1 ml of vitamin K was injected intramuscularly (group 7) as reference drug to seventh the group. Twelve male rats were assigned into two equal groups (n = 6/gp), 2 ml of distilled water (DW) and doses of DE (1500 mg/kg) were orally administered. Clotting time was determined on the Days 1, 2, and 7 using Lee and White method. In the DE treated groups with all doses, there was no reduction in clotting time on the Day 1 but a significant reduction of clotting time (P dulcis has proclotting activity (rakthasthambhana property) and this was faster than vitamin K.

  7. Softcopy quality ruler method: implementation and validation

    Science.gov (United States)

    Jin, Elaine W.; Keelan, Brian W.; Chen, Junqing; Phillips, Jonathan B.; Chen, Ying

    2009-01-01

    A softcopy quality ruler method was implemented for the International Imaging Industry Association (I3A) Camera Phone Image Quality (CPIQ) Initiative. This work extends ISO 20462 Part 3 by virtue of creating reference digital images of known subjective image quality, complimenting the hardcopy Standard Reference Stimuli (SRS). The softcopy ruler method was developed using images from a Canon EOS 1Ds Mark II D-SLR digital still camera (DSC) and a Kodak P880 point-and-shoot DSC. Images were viewed on an Apple 30in Cinema Display at a viewing distance of 34 inches. Ruler images were made for 16 scenes. Thirty ruler images were generated for each scene, representing ISO 20462 Standard Quality Scale (SQS) values of approximately 2 to 31 at an increment of one just noticeable difference (JND) by adjusting the system modulation transfer function (MTF). A Matlab GUI was developed to display the ruler and test images side-by-side with a user-adjustable ruler level controlled by a slider. A validation study was performed at Kodak, Vista Point Technology, and Aptina Imaging in which all three companies set up a similar viewing lab to run the softcopy ruler method. The results show that the three sets of data are in reasonable agreement with each other, with the differences within the range expected from observer variability. Compared to previous implementations of the quality ruler, the slider-based user interface allows approximately 2x faster assessments with 21.6% better precision.

  8. Development and implementation of tPA clot lysis activity assay using ACL TOP™ hemeostasis testing system in QC laboratories

    Directory of Open Access Journals (Sweden)

    Lichun Huang

    2017-12-01

    Full Text Available This report describes the design, development, validation and long-term performance of tPA clot lysis activity assay using Advanced Chemistry Line Total Operational Performance (ACL TOP™ Homeostasis Testing System. The results of the study demonstrated robust and stable performance of the analytical method. The accuracy of the assay, expressed by percent recovery is 98–99%. The intermediate precision and repeatability precision, expressed as Relative Standard Deviation (RSD, was 3% and less than 2% respectively. The validated range is from 70% to 130% of the target potency of 5.8 × 105 IU/mg. The linearity of this range, expressed in correlation coefficient, is 0.997. After the assay is transferred to a QC laboratory, the assay retained high accuracy and precision with a success rate of >99%. Keywords: Potency assay, Clot lysis, Comparability, Automation

  9. 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.

  10. Ultrastructure of clots during isometric contraction

    OpenAIRE

    1982-01-01

    We explored the retraction or contraction of platelet-fibrin clots under isometric conditions. In the presence of micromolar calcium clots of normal platelet-rich plasma developed tension at an initial rate of 0.1 to 0.2 g/min per cm2 (initial cross-sectional area). Electron microscopy of clots fixed after attaining a force of 1.6 g/cm2 revealed platelets with elongated bodies and pseudopods in close apposition to fibrin strands which were oriented in cablelike fashion in the direction of ten...

  11. 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…

  12. FDIR Strategy Validation with the B Method

    Science.gov (United States)

    Sabatier, D.; Dellandrea, B.; Chemouil, D.

    2008-08-01

    In a formation flying satellite system, the FDIR strategy (Failure Detection, Isolation and Recovery) is paramount. When a failure occurs, satellites should be able to take appropriate reconfiguration actions to obtain the best possible results given the failure, ranging from avoiding satellite-to-satellite collision to continuing the mission without disturbance if possible. To achieve this goal, each satellite in the formation has an implemented FDIR strategy that governs how it detects failures (from tests or by deduction) and how it reacts (reconfiguration using redundant equipments, avoidance manoeuvres, etc.). The goal is to protect the satellites first and the mission as much as possible. In a project initiated by the CNES, ClearSy experiments the B Method to validate the FDIR strategies developed by Thales Alenia Space, of the inter satellite positioning and communication devices that will be used for the SIMBOL-X (2 satellite configuration) and the PEGASE (3 satellite configuration) missions and potentially for other missions afterward. These radio frequency metrology sensor devices provide satellite positioning and inter satellite communication in formation flying. This article presents the results of this experience.

  13. Analytical difficulties facing today's regulatory laboratories: issues in method validation.

    Science.gov (United States)

    MacNeil, James D

    2012-08-01

    The challenges facing analytical laboratories today are not unlike those faced in the past, although both the degree of complexity and the rate of change have increased. Challenges such as development and maintenance of expertise, maintenance and up-dating of equipment, and the introduction of new test methods have always been familiar themes for analytical laboratories, but international guidelines for laboratories involved in the import and export testing of food require management of such changes in a context which includes quality assurance, accreditation, and method validation considerations. Decisions as to when a change in a method requires re-validation of the method or on the design of a validation scheme for a complex multi-residue method require a well-considered strategy, based on a current knowledge of international guidance documents and regulatory requirements, as well the laboratory's quality system requirements. Validation demonstrates that a method is 'fit for purpose', so the requirement for validation should be assessed in terms of the intended use of a method and, in the case of change or modification of a method, whether that change or modification may affect a previously validated performance characteristic. In general, method validation involves method scope, calibration-related parameters, method precision, and recovery. Any method change which may affect method scope or any performance parameters will require re-validation. Some typical situations involving change in methods are discussed and a decision process proposed for selection of appropriate validation measures. © 2012 John Wiley & Sons, Ltd.

  14. Development and Validation of a Dissolution Test Method for ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a dissolution test method for dissolution release of artemether and lumefantrine from tablets. Methods: A single dissolution method for evaluating the in vitro release of artemether and lumefantrine from tablets was developed and validated. The method comprised of a dissolution medium of ...

  15. 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…

  16. Method validation in pharmaceutical analysis: from theory to practical optimization

    Directory of Open Access Journals (Sweden)

    Jaqueline Kaleian Eserian

    2015-01-01

    Full Text Available The validation of analytical methods is required to obtain high-quality data. For the pharmaceutical industry, method validation is crucial to ensure the product quality as regards both therapeutic efficacy and patient safety. The most critical step in validating a method is to establish a protocol containing well-defined procedures and criteria. A well planned and organized protocol, such as the one proposed in this paper, results in a rapid and concise method validation procedure for quantitative high performance liquid chromatography (HPLC analysis.   Type: Commentary

  17. Effects of botropase on clotting factors in healthy human volunteers

    Directory of Open Access Journals (Sweden)

    Ashok K Shenoy

    2014-01-01

    Full Text Available Objective: To evaluate the effects of botropase on various clotting factors in human volunteers. Materials and Methods: It was a prospective open label study conducted on human healthy volunteers. After the baseline screening, subjects fulfilling inclusion criteria were enrolled. On the study day, 1 ml of botropase was administered intravenously and after an hour same dose of botropase (1 ml was given by intramuscular (IM route. The efficacy and safety parameters were monitored up to 72 h from the time of intravenous (IV administration. Results: A total of 15 volunteers, belonging to 24-35 years of age were included in the study. Botropase significantly reduced the plasma level of fibrinogen and fibrin degradation products after 5 min of IV administration (P < 0.05. In addition, factor X was observed to reduce constantly by botropase administration suggesting enhanced turnover between 5 and 20 min of IV administration. Although botropase reduced clotting and bleeding time in all the volunteers, the data remains to be statistically insignificant. Conclusion: Present study demonstrated the safety and efficacy of botropase in human healthy volunteers. The study has shown that it is a factor X activator and reduces effectively clotting and bleeding time.

  18. The Phosphatase Inhibitor Calyculin-A Impairs Clot Retraction, Platelet Activation, and Thrombin Generation

    Directory of Open Access Journals (Sweden)

    Renáta Hudák

    2017-01-01

    Full Text Available The aim of this study was to investigate the effect of the serine/threonine protein phosphatase inhibitor, calyculin-A (CLA, on clot formation and on the procoagulant activity of human platelets. Platelet-rich plasma (PRP samples were preincubated with buffer or CLA and subsequently platelets were activated by the protease-activated receptor 1 (PAR-1 activator, thrombin receptor activating peptide (TRAP. Clot retraction was detected by observing clot morphology up to 1 hour, phosphatidylserine- (PS- expression was studied by flow cytometry, and thrombin generation was measured by a fluorimetric assay. For the intracellular Ca2+ assay, platelets were loaded with calcium-indicator dyes and the measurements were carried out using a ratiometric method with real-time confocal microscopy. CLA preincubation inhibited clot retraction, PS-expression, and thrombin formation. TRAP activation elicited Ca2+ response and PS-expression in a subset of platelets. The activated PRP displayed significantly faster and enhanced thrombin generation compared to nonactivated samples. CLA pretreatment abrogated PS-exposure and clot retraction also in TRAP-activated samples. As a consequence of the inhibitory effect on calcium elevation and PS-expression, CLA significantly downregulated thrombin generation in PRP. Our results show that CLA pretreatment may be a useful tool to investigate platelet activation mechanisms that contribute to clot formation and thrombin generation.

  19. Development and validation of a spectroscopic method for the ...

    African Journals Online (AJOL)

    Development and validation of a spectroscopic method for the simultaneous analysis of ... advanced analytical methods such as high pressure liquid ..... equipment. DECLARATIONS ... high-performance liquid chromatography. J Chromatogr.

  20. Measuring factor IX activity of nonacog beta pegol with commercially available one-stage clotting and chromogenic assay kits: a two-center study.

    Science.gov (United States)

    Bowyer, A E; Hillarp, A; Ezban, M; Persson, P; Kitchen, S

    2016-07-01

    Essentials Validated assays are required to precisely measure factor IX (FIX) activity in FIX products. N9-GP and two other FIX products were assessed in various coagulation assay systems at two sites. Large variations in FIX activity measurements were observed for N9-GP using some assays. One-stage and chromogenic assays accurately measuring FIX activity for N9-GP were identified. Background Measurement of factor IX activity (FIX:C) with activated partial thromboplastin time-based one-stage clotting assays is associated with a large degree of interlaboratory variation in samples containing glycoPEGylated recombinant FIX (rFIX), i.e. nonacog beta pegol (N9-GP). Validation and qualification of specific assays and conditions are necessary for the accurate assessment of FIX:C in samples containing N9-GP. Objectives To assess the accuracy of various one-stage clotting and chromogenic assays for measuring FIX:C in samples containing N9-GP as compared with samples containing rFIX or plasma-derived FIX (pdFIX) across two laboratory sites. Methods FIX:C, in severe hemophilia B plasma spiked with a range of concentrations (from very low, i.e. 0.03 IU mL(-1) , to high, i.e. 0.90 IU mL(-1) ) of N9-GP, rFIX (BeneFIX), and pdFIX (Mononine), was determined at two laboratory sites with 10 commercially available one-stage clotting assays and two chromogenic FIX:C assays. Assays were performed with a plasma calibrator and different analyzers. Results A high degree of variation in FIX:C measurement was observed for one-stage clotting assays for N9-GP as compared with rFIX or pdFIX. Acceptable N9-GP recovery was observed in the low-concentration to high-concentration samples tested with one-stage clotting assays using SynthAFax or DG Synth, or with chromogenic FIX:C assays. Similar patterns of FIX:C measurement were observed at both laboratory sites, with minor differences probably being attributable to the use of different analyzers. Conclusions These results suggest that, of the

  1. Validation of method in instrumental NAA for food products sample

    International Nuclear Information System (INIS)

    Alfian; Siti Suprapti; Setyo Purwanto

    2010-01-01

    NAA is a method of testing that has not been standardized. To affirm and confirm that this method is valid. it must be done validation of the method with various sample standard reference materials. In this work. the validation is carried for food product samples using NIST SRM 1567a (wheat flour) and NIST SRM 1568a (rice flour). The results show that the validation method for testing nine elements (Al, K, Mg, Mn, Na, Ca, Fe, Se and Zn) in SRM 1567a and eight elements (Al, K, Mg, Mn, Na, Ca, Se and Zn ) in SRM 1568a pass the test of accuracy and precision. It can be conclude that this method has power to give valid result in determination element of the food products samples. (author)

  2. Validated High Performance Liquid Chromatography Method for ...

    African Journals Online (AJOL)

    Purpose: To develop a simple, rapid and sensitive high performance liquid chromatography (HPLC) method for the determination of cefadroxil monohydrate in human plasma. Methods: Schimadzu HPLC with LC solution software was used with Waters Spherisorb, C18 (5 μm, 150mm × 4.5mm) column. The mobile phase ...

  3. Human Factors methods concerning integrated validation of nuclear power plant control rooms; Metodutveckling foer integrerad validering

    Energy Technology Data Exchange (ETDEWEB)

    Oskarsson, Per-Anders; Johansson, Bjoern J.E.; Gonzalez, Natalia (Swedish Defence Research Agency, Information Systems, Linkoeping (Sweden))

    2010-02-15

    The frame of reference for this work was existing recommendations and instructions from the NPP area, experiences from the review of the Turbic Validation and experiences from system validations performed at the Swedish Armed Forces, e.g. concerning military control rooms and fighter pilots. These enterprises are characterized by complex systems in extreme environments, often with high risks, where human error can lead to serious consequences. A focus group has been performed with representatives responsible for Human Factors issues from all Swedish NPP:s. The questions that were discussed were, among other things, for whom an integrated validation (IV) is performed and its purpose, what should be included in an IV, the comparison with baseline measures, the design process, the role of SSM, which methods of measurement should be used, and how the methods are affected of changes in the control room. The report brings different questions to discussion concerning the validation process. Supplementary methods of measurement for integrated validation are discussed, e.g. dynamic, psychophysiological, and qualitative methods for identification of problems. Supplementary methods for statistical analysis are presented. The study points out a number of deficiencies in the validation process, e.g. the need of common guidelines for validation and design, criteria for different types of measurements, clarification of the role of SSM, and recommendations for the responsibility of external participants in the validation process. The authors propose 12 measures for taking care of the identified problems

  4. Validated high performance liquid chromatographic (HPLC) method ...

    African Journals Online (AJOL)

    STORAGESEVER

    2010-02-22

    Feb 22, 2010 ... specific and accurate high performance liquid chromatographic method for determination of ZER in micro-volumes ... tional medicine as a cure for swelling, sores, loss of appetite and ... Receptor Activator for Nuclear Factor κ B Ligand .... The effect of ... be suitable for preclinical pharmacokinetic studies. The.

  5. 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

  6. Validation Method of a Telecommunications Blackout Attack

    National Research Council Canada - National Science Library

    Amado, Joao; Nunes, Paulo

    2005-01-01

    ..., and to obtain the maximum disruptive effect over the services. The proposed method uses a top-down approach, starting on the service level and ending on the different network elements that can be identified in the end as the targets for the attack.

  7. Valid methods: the quality assurance of test method development, validation, approval, and transfer for veterinary testing laboratories.

    Science.gov (United States)

    Wiegers, Ann L

    2003-07-01

    Third-party accreditation is a valuable tool to demonstrate a laboratory's competence to conduct testing. Accreditation, internationally and in the United States, has been discussed previously. However, accreditation is only I part of establishing data credibility. A validated test method is the first component of a valid measurement system. Validation is defined as confirmation by examination and the provision of objective evidence that the particular requirements for a specific intended use are fulfilled. The international and national standard ISO/IEC 17025 recognizes the importance of validated methods and requires that laboratory-developed methods or methods adopted by the laboratory be appropriate for the intended use. Validated methods are therefore required and their use agreed to by the client (i.e., end users of the test results such as veterinarians, animal health programs, and owners). ISO/IEC 17025 also requires that the introduction of methods developed by the laboratory for its own use be a planned activity conducted by qualified personnel with adequate resources. This article discusses considerations and recommendations for the conduct of veterinary diagnostic test method development, validation, evaluation, approval, and transfer to the user laboratory in the ISO/IEC 17025 environment. These recommendations are based on those of nationally and internationally accepted standards and guidelines, as well as those of reputable and experienced technical bodies. They are also based on the author's experience in the evaluation of method development and transfer projects, validation data, and the implementation of quality management systems in the area of method development.

  8. Limitations of using synthetic blood clots for measuring in vitro clot capture efficiency of inferior vena cava filters

    Directory of Open Access Journals (Sweden)

    Robinson RA

    2013-05-01

    Full Text Available Ronald A Robinson, Luke H Herbertson, Srilekha Sarkar Das, Richard A Malinauskas, William F Pritchard, Laurence W GrossmanOffice of Science and Engineering Laboratories, Center for Devices and Radiological Health, US Food and Drug Administration, Silver Spring, MD, USAAbstract: The purpose of this study was first to evaluate the clot capture efficiency and capture location of six currently-marketed vena cava filters in a physiological venous flow loop, using synthetic polyacrylamide hydrogel clots, which were intended to simulate actual blood clots. After observing a measured anomaly for one of the test filters, we redirected the focus of the study to identify the cause of poor clot capture performance for large synthetic hydrogel clots. We hypothesized that the uncharacteristic low clot capture efficiency observed when testing the outlying filter can be attributed to the inadvertent use of dense, stiff synthetic hydrogel clots, and not as a result of the filter design or filter orientation. To study this issue, sheep blood clots and polyacrylamide (PA synthetic clots were injected into a mock venous flow loop containing a clinical inferior vena cava (IVC filter, and their captures were observed. Testing was performed with clots of various diameters (3.2, 4.8, and 6.4 mm, length-to-diameter ratios (1:1, 3:1, 10:1, and stiffness. By adjusting the chemical formulation, PA clots were fabricated to be soft, moderately stiff, or stiff with elastic moduli of 805 ± 2, 1696 ± 10 and 3295 ± 37 Pa, respectively. In comparison, the elastic moduli for freshly prepared sheep blood clots were 1690 ± 360 Pa. The outlying filter had a design that was characterized by peripheral gaps (up to 14 mm between its wire struts. While a low clot capture rate was observed using large, stiff synthetic clots, the filter effectively captured similarly sized sheep blood clots and soft PA clots. Because the stiffer synthetic clots remained straight when approaching the

  9. A preliminary investigation of PSA validation methods

    Energy Technology Data Exchange (ETDEWEB)

    Unwin, S D [Science Applications International Corp., (United States)

    1995-09-01

    This document has been prepared to support the initial phase of the Atomic Energy Control Board`s program to review and evaluate Probabilistic Safety Assessment (PSA) studies conducted by nuclear generating station designers and licensees. The document provides (1) a review of current and prospective applications of PSA technology in the Canadian nuclear power industry; (2) an assessment of existing practices and techniques for the review or risk and hazard identification studies in the international nuclear power sector and other technological sectors; and (3) proposed analytical framework in which to develop systematic techniques for the scrutiny and evaluation of a PSA model. These frameworks are based on consideration of the mathematical structure of a PSA model and are intended to facilitate the development of methods to evaluate a model relative to intended end-uses. (author). 34 refs., 10 tabs., 3 figs.

  10. A preliminary investigation of PSA validation methods

    International Nuclear Information System (INIS)

    Unwin, S.D.

    1995-09-01

    This document has been prepared to support the initial phase of the Atomic Energy Control Board's program to review and evaluate Probabilistic Safety Assessment (PSA) studies conducted by nuclear generating station designers and licensees. The document provides (1) a review of current and prospective applications of PSA technology in the Canadian nuclear power industry; (2) an assessment of existing practices and techniques for the review or risk and hazard identification studies in the international nuclear power sector and other technological sectors; and (3) proposed analytical framework in which to develop systematic techniques for the scrutiny and evaluation of a PSA model. These frameworks are based on consideration of the mathematical structure of a PSA model and are intended to facilitate the development of methods to evaluate a model relative to intended end-uses. (author). 34 refs., 10 tabs., 3 figs

  11. 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......) and determination of the content by gas chromatography (GC) with electron capture (EC-), nitrogen/phosphorous (NP-), and mass spectrometric (MS-) detection. Three strobilurins, azoxystrobin, kresoxim-methyl and trifloxystrobin were validated on three matrices, wheat, apple and grapes. The validation was based...

  12. A novel clot lysis assay for recombinant plasminogen activator.

    Science.gov (United States)

    Jamialahmadi, Oveis; Fazeli, Ahmad; Hashemi-Najafabadi, Sameereh; Fazeli, Mohammad Reza

    2015-03-01

    Recombinant plasminogen activator (r-PA, reteplase) is an engineered variant of alteplase. When expressed in E. coli, it appears as inclusion bodies that require refolding to recover its biological activity. An important step following refolding is to determine the activity of refolded protein. Current methods for enzymatic activity of thrombolytic drugs are costly and complex. Here a straightforward and low-cost clot lysis assay was developed. It quantitatively measures the activity of the commercial reteplase and is also capable of screening refolding conditions. As evidence for adequate accuracy and sensitivity of the current assay, r-PA activity measurements are shown to be comparable to those obtained from chromogenic substrate assay.

  13. International Harmonization and Cooperation in the Validation of Alternative Methods.

    Science.gov (United States)

    Barroso, João; Ahn, Il Young; Caldeira, Cristiane; Carmichael, Paul L; Casey, Warren; Coecke, Sandra; Curren, Rodger; Desprez, Bertrand; Eskes, Chantra; Griesinger, Claudius; Guo, Jiabin; Hill, Erin; Roi, Annett Janusch; Kojima, Hajime; Li, Jin; Lim, Chae Hyung; Moura, Wlamir; Nishikawa, Akiyoshi; Park, HyeKyung; Peng, Shuangqing; Presgrave, Octavio; Singer, Tim; Sohn, Soo Jung; Westmoreland, Carl; Whelan, Maurice; Yang, Xingfen; Yang, Ying; Zuang, Valérie

    The development and validation of scientific alternatives to animal testing is important not only from an ethical perspective (implementation of 3Rs), but also to improve safety assessment decision making with the use of mechanistic information of higher relevance to humans. To be effective in these efforts, it is however imperative that validation centres, industry, regulatory bodies, academia and other interested parties ensure a strong international cooperation, cross-sector collaboration and intense communication in the design, execution, and peer review of validation studies. Such an approach is critical to achieve harmonized and more transparent approaches to method validation, peer-review and recommendation, which will ultimately expedite the international acceptance of valid alternative methods or strategies by regulatory authorities and their implementation and use by stakeholders. It also allows achieving greater efficiency and effectiveness by avoiding duplication of effort and leveraging limited resources. In view of achieving these goals, the International Cooperation on Alternative Test Methods (ICATM) was established in 2009 by validation centres from Europe, USA, Canada and Japan. ICATM was later joined by Korea in 2011 and currently also counts with Brazil and China as observers. This chapter describes the existing differences across world regions and major efforts carried out for achieving consistent international cooperation and harmonization in the validation and adoption of alternative approaches to animal testing.

  14. 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)

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

    International Nuclear Information System (INIS)

    Petroni, Robson; Moreira, Edson G.

    2015-01-01

    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)

  16. Testing and Validation of Computational Methods for Mass Spectrometry.

    Science.gov (United States)

    Gatto, Laurent; Hansen, Kasper D; Hoopmann, Michael R; Hermjakob, Henning; Kohlbacher, Oliver; Beyer, Andreas

    2016-03-04

    High-throughput methods based on mass spectrometry (proteomics, metabolomics, lipidomics, etc.) produce a wealth of data that cannot be analyzed without computational methods. The impact of the choice of method on the overall result of a biological study is often underappreciated, but different methods can result in very different biological findings. It is thus essential to evaluate and compare the correctness and relative performance of computational methods. The volume of the data as well as the complexity of the algorithms render unbiased comparisons challenging. This paper discusses some problems and challenges in testing and validation of computational methods. We discuss the different types of data (simulated and experimental validation data) as well as different metrics to compare methods. We also introduce a new public repository for mass spectrometric reference data sets ( http://compms.org/RefData ) that contains a collection of publicly available data sets for performance evaluation for a wide range of different methods.

  17. Massive clot formation after tooth extraction

    Directory of Open Access Journals (Sweden)

    Santosh Hunasgi

    2015-01-01

    Full Text Available Oral surgical procedures mainly tooth extraction can be related with an extended hemorrhage owed to the nature of the process resulting in an "open wound." The attempt of this paper is to present a case of massive postoperative clot formation after tooth extraction and highlight on the oral complications of surgical procedures. A 32-year-old male patient reported to the Dental Clinic for evaluation and extraction of grossly decayed 46. Clinical evaluation of 46 revealed root stumps. Extraction of the root stumps was performed, and it was uneventful. Hemostasis was achieved and postsurgical instructions were specified to the patient. The patient reported to the clinic, the very subsequent morning with a criticism of bleeding at the extraction site. On clinical examination, bleeding was noted from the socket in relation to 46. To control bleeding, oral hemostatic drugs Revici - E (Ethamsylate 500 mg was prescribed and bleeding was stopped in 2 h. However, a massive clot was formed at the extraction site. Further, this clot resolved on its own in 1-week time. Despite the fact that dental extraction is considered to be a minor surgical procedure, some cases may present with life-threatening complications including hemorrhage. Vigilant and significant history taking, physical and dental examinations prior to dental procedures are a must to avoid intraoperative and postoperative complications.

  18. Development and Validation of Improved Method for Fingerprint ...

    African Journals Online (AJOL)

    Purpose: To develop and validate an improved method by capillary zone electrophoresis with photodiode array detection for the fingerprint analysis of Ligusticum chuanxiong Hort. (Rhizoma Chuanxiong). Methods: The optimum high performance capillary electrophoresis (HPCE) conditions were 30 mM borax containing 5 ...

  19. Development and Validation of a Bioanalytical Method for Direct ...

    African Journals Online (AJOL)

    Purpose: To develop and validate a user-friendly spiked plasma method for the extraction of diclofenac potassium that reduces the number of treatments with plasma sample, in order to minimize human error. Method: Instead of solvent evaporation technique, the spiked plasma sample was modified with H2SO4 and NaCl, ...

  20. Development and Validation of Analytical Method for Losartan ...

    African Journals Online (AJOL)

    Development and Validation of Analytical Method for Losartan-Copper Complex Using UV-Vis Spectrophotometry. ... Tropical Journal of Pharmaceutical Research ... Purpose: To develop a new spectrophotometric method for the analysis of losartan potassium in pharmaceutical formulations by making its complex with ...

  1. 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…

  2. Validation of Land Cover Products Using Reliability Evaluation Methods

    Directory of Open Access Journals (Sweden)

    Wenzhong Shi

    2015-06-01

    Full Text Available Validation of land cover products is a fundamental task prior to data applications. Current validation schemes and methods are, however, suited only for assessing classification accuracy and disregard the reliability of land cover products. The reliability evaluation of land cover products should be undertaken to provide reliable land cover information. In addition, the lack of high-quality reference data often constrains validation and affects the reliability results of land cover products. This study proposes a validation schema to evaluate the reliability of land cover products, including two methods, namely, result reliability evaluation and process reliability evaluation. Result reliability evaluation computes the reliability of land cover products using seven reliability indicators. Process reliability evaluation analyzes the reliability propagation in the data production process to obtain the reliability of land cover products. Fuzzy fault tree analysis is introduced and improved in the reliability analysis of a data production process. Research results show that the proposed reliability evaluation scheme is reasonable and can be applied to validate land cover products. Through the analysis of the seven indicators of result reliability evaluation, more information on land cover can be obtained for strategic decision-making and planning, compared with traditional accuracy assessment methods. Process reliability evaluation without the need for reference data can facilitate the validation and reflect the change trends of reliabilities to some extent.

  3. 76 FR 28664 - Method 301-Field Validation of Pollutant Measurement Methods From Various Waste Media

    Science.gov (United States)

    2011-05-18

    ... . d m = The mean of the paired sample differences. n = Total number of paired samples. 7.4.2 t Test... being compared to a validated test method as part of the Method 301 validation and an audit sample for... tighten the acceptance criteria for the precision of candidate alternative test methods. One commenter...

  4. Formation of blood clot on biomaterial implants influences bone healing.

    Science.gov (United States)

    Shiu, Hoi Ting; Goss, Ben; Lutton, Cameron; Crawford, Ross; Xiao, Yin

    2014-12-01

    The first step in bone healing is forming a blood clot at injured bones. During bone implantation, biomaterials unavoidably come into direct contact with blood, leading to a blood clot formation on its surface prior to bone regeneration. Despite both situations being similar in forming a blood clot at the defect site, most research in bone tissue engineering virtually ignores the important role of a blood clot in supporting healing. Dental implantology has long demonstrated that the fibrin structure and cellular content of a peri-implant clot can greatly affect osteoconduction and de novo bone formation on implant surfaces. This article reviews the formation of a blood clot during bone healing in relation to the use of platelet-rich plasma (PRP) gels. It is implicated that PRP gels are dramatically altered from a normal clot in healing, resulting in conflicting effect on bone regeneration. These results indicate that the effect of clots on bone regeneration depends on how the clots are formed. Factors that influence blood clot structure and properties in relation to bone healing are also highlighted. Such knowledge is essential for developing strategies to optimally control blood clot formation, which ultimately alter the healing microenvironment of bone. Of particular interest are modification of surface chemistry of biomaterials, which displays functional groups at varied composition for the purpose of tailoring blood coagulation activation, resultant clot fibrin architecture, rigidity, susceptibility to lysis, and growth factor release. This opens new scope of in situ blood clot modification as a promising approach in accelerating and controlling bone regeneration.

  5. Validation of NAA Method for Urban Particulate Matter

    International Nuclear Information System (INIS)

    Woro Yatu Niken Syahfitri; Muhayatun; Diah Dwiana Lestiani; Natalia Adventini

    2009-01-01

    Nuclear analytical techniques have been applied in many countries for determination of environmental pollutant. Method of NAA (neutron activation analysis) representing one of nuclear analytical technique of that has low detection limits, high specificity, high precision, and accuracy for large majority of naturally occurring elements, and ability of non-destructive and simultaneous determination of multi-elemental, and can handle small sample size (< 1 mg). To ensure quality and reliability of the method, validation are needed to be done. A standard reference material, SRM NIST 1648 Urban Particulate Matter, has been used to validate NAA method. Accuracy and precision test were used as validation parameters. Particulate matter were validated for 18 elements: Ti, I, V, Br, Mn, Na, K, Cl, Cu, Al, As, Fe, Co, Zn, Ag, La, Cr, and Sm,. The result showed that the percent relative standard deviation of the measured elemental concentrations are found to be within ranged from 2 to 14,8% for most of the elements analyzed whereas Hor rat value in range 0,3-1,3. Accuracy test results showed that relative bias ranged from -11,1 to 3,6%. Based on validation results, it can be stated that NAA method is reliable for characterization particulate matter and other similar matrix samples to support air quality monitoring. (author)

  6. Validation of calculational methods for nuclear criticality safety - approved 1975

    International Nuclear Information System (INIS)

    Anon.

    1977-01-01

    The American National Standard for Nuclear Criticality Safety in Operations with Fissionable Materials Outside Reactors, N16.1-1975, states in 4.2.5: In the absence of directly applicable experimental measurements, the limits may be derived from calculations made by a method shown to be valid by comparison with experimental data, provided sufficient allowances are made for uncertainties in the data and in the calculations. There are many methods of calculation which vary widely in basis and form. Each has its place in the broad spectrum of problems encountered in the nuclear criticality safety field; however, the general procedure to be followed in establishing validity is common to all. The standard states the requirements for establishing the validity and area(s) of applicability of any calculational method used in assessing nuclear criticality safety

  7. High-Quality and -Quantity DNA Extraction from Frozen Archival Blood Clots for Genotyping of Single-Nucleotide Polymorphisms

    DEFF Research Database (Denmark)

    Bank, Steffen; Nexø, Bjørn Andersen; Andersen, Vibeke

    2013-01-01

    the efficiency of commercial purification kits for extracting DNA from long-term frozen clotted blood. Methods: Serum tubes with clotted blood were stored at −20°C for 1 to 2.5 years before DNA extraction. DNA was extracted from 10 blood clot samples using PureGene (Qiagen) with and without glycogen, the QIAamp...... with a median of 0.65 μg (range 0.5–2.6 μg) pr 300 μL total blood. Conclusion: The yield obtained by the different commercial kits varied considerably. Our work demonstrates that high-quality and -quantity DNA can be extracted with the Maxwell 16 Blood purification kit (Promega) from cryopreserved blood clots...

  8. Development and Validation of a Liquid Chromatographic Method ...

    African Journals Online (AJOL)

    A liquid chromatographic method for the simultaneous determination of six human immunodeficiency virus (HIV) protease inhibitors, indinavir, saquinavir, ritonavir, amprenavir, nelfinavir and lopinavir, was developed and validated. Optimal separation was achieved on a PLRP-S 100 Å, 250 x 4.6 mm I.D. column maintained ...

  9. Validated RP-HPLC Method for Quantification of Phenolic ...

    African Journals Online (AJOL)

    Purpose: To evaluate the total phenolic content and antioxidant potential of the methanol extracts of aerial parts and roots of Thymus sipyleus Boiss and also to determine some phenolic compounds using a newly developed and validated reversed phase high performance liquid chromatography (RP-HPLC) method.

  10. Comparison of the performances and validation of three methods for ...

    African Journals Online (AJOL)

    SARAH

    2014-02-28

    Feb 28, 2014 ... bacteria in Norwegian slaughter pigs. Int J. Food Microbiol 1, 301–309. [NCFA] Nordic Committee of Food Analysis (1996). Yersinia enterocolitica Detection in foods 117,. 3rd,edn,1-12. Nowak, B., Mueffling, T.V., Caspari, K. and Hartung, J. 2006 Validation of a method for the detection of virulent Yersinia ...

  11. Development and validation of analytical methods for dietary supplements

    International Nuclear Information System (INIS)

    Sullivan, Darryl; Crowley, Richard

    2006-01-01

    The expanding use of innovative botanical ingredients in dietary supplements and foods has resulted in a flurry of research aimed at the development and validation of analytical methods for accurate measurement of active ingredients. The pressing need for these methods is being met through an expansive collaborative initiative involving industry, government, and analytical organizations. This effort has resulted in the validation of several important assays as well as important advances in the method engineering procedures which have improved the efficiency of the process. The initiative has also allowed researchers to hurdle many of the barricades that have hindered accurate analysis such as the lack of reference standards and comparative data. As the availability for nutraceutical products continues to increase these methods will provide consumers and regulators with the scientific information needed to assure safety and dependable labeling

  12. Honey Bee Venom (Apis mellifera Contains Anticoagulation Factors and Increases the Blood-clotting Time

    Directory of Open Access Journals (Sweden)

    Hossein Zolfagharian

    2015-12-01

    Full Text Available Objectives: Bee venom (BV is a complex mixture of proteins and contains proteins such as phospholipase and melittin, which have an effect on blood clotting and blood clots. The mechanism of action of honey bee venom (HBV, Apis mellifera on human plasma proteins and its anti-thrombotic effect were studied. The purpose of this study was to investigate the anti-coagulation effect of BV and its effects on blood coagulation and purification. Methods: Crude venom obtained from Apis mellifera was selected. The anti-coagulation factor of the crude venom from this species was purified by using gel filtration chromatography (sephadex G-50, and the molecular weights of the anti-coagulants in this venom estimated by using sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE. Blood samples were obtained from 10 rabbits, and the prothrombin time (PT and the partial thromboplastin time (PTT tests were conducted. The approximate lethal dose (LD values of BV were determined. Results: Crude BV increased the blood clotting time. For BV concentrations from 1 to 4 mg/mL, clotting was not observed even at more than 300 seconds, standard deviations (SDs = ± 0.71; however, clotting was observed in the control group 13.8 s, SDs = ± 0.52. Thus, BV can be considered as containing anti-coagulation factors. Crude BV is composed 4 protein bands with molecular weights of 3, 15, 20 and 41 kilodalton (kDa, respectively. The LD50 of the crude BV was found to be 177.8 μg/mouse. Conclusion: BV contains anti-coagulation factors. The fraction extracted from the Iranian bees contains proteins that are similar to anti-coagulation proteins, such as phospholipase A2 (PLA2 and melittin, and that can increase the blood clotting times in vitro.

  13. The Validity of Dimensional Regularization Method on Fractal Spacetime

    Directory of Open Access Journals (Sweden)

    Yong Tao

    2013-01-01

    Full Text Available Svozil developed a regularization method for quantum field theory on fractal spacetime (1987. Such a method can be applied to the low-order perturbative renormalization of quantum electrodynamics but will depend on a conjectural integral formula on non-integer-dimensional topological spaces. The main purpose of this paper is to construct a fractal measure so as to guarantee the validity of the conjectural integral formula.

  14. Pre-analytical variation in glucose concentration due to atmospheric temperature and clot in blood specimens

    International Nuclear Information System (INIS)

    Butt, T.; Masud, K.; Khan, J.A.; Bhatti, M.S.

    2016-01-01

    Objective: To determine the effect of temperature and contact of clot with serum on laboratory results of glucose concentration in blood. Study Design: Quasi-experimental study. Place and Duration of Study: December 2014 to August 2015 at the laboratory of Shoaib Hospital, Fateh Jang, Attock Pakistan. Material and Methods: Samples were collected for estimation of blood glucose (Random) concentration from patients reporting to the hospital. Blood specimens (n=94) of such volunteers were analyzed for glucose level. Each sample was put up in five tubes. When the blood clotted the serum from tube-1 was analyzed for glucose level within 30 minutes. In tube-2 and tube-3 serum was kept for 24 hours at room temperature and refrigerator temperature respectively before glucose estimation. In tube-4 and tube-5 serum was not separated from clot and kept at room temperature and refrigerator temperature respectively before glucose estimation. The value of tube 1 was taken as reference value for comparison with other parts of the specimen. The equipment used for blood glucose level estimation was semi auto chemistry analyzer (Rayto, China). The kit used for analysis was Glucose - Liquizyme (Germany). Results: The difference between the mean reference value (tube-1) and refrigerated serum without clot (tube-3) was 4.63 mg/100 ml while that of unrefrigerated portion (tube-2) had a difference of 10.68 mg/100 ml. The mean of unrefrigerated (tube-4) and refrigerated (tube-5) portions of serum kept with the clot had difference of 42.05 mg/100 ml and 25.84 mg/100 ml respectively. The fall in the blood glucose level in all (n=94) the samples in the tube number 3 (serum separated and kept at refrigerated temperature) was 4.63 mg/100 ml +- 3.68 (Mean +- SD) and it ranged from 0 to 20 mg/100 ml whereas fall was maximum in the tube number 4 (serum with clotted blood and kept at room temperature) was 42.04 mg/100 ml +- 10.61 (Mean +- SD) and it ranged from 13 to 82 mg/100 ml. The sample in

  15. Identification of quantitative trait loci for fibrin clot phenotypes: the EuroCLOT study

    DEFF Research Database (Denmark)

    Williams, Frances M K; Carter, Angela M; Kato, Bernet

    2009-01-01

    OBJECTIVE: Fibrin makes up the structural basis of an occlusive arterial thrombus, and variability in fibrin phenotype relates to cardiovascular risk. The aims of the current study from the EU consortium EuroCLOT were to (1) determine the heritability of fibrin phenotypes and (2) identify QTLs as...

  16. The effects of Aloe vera [gel] on clotting time, prothrombin time and ...

    African Journals Online (AJOL)

    Background: Published reports on the effects of Aloe vera gel on blood coagulation in experimental animals are relatively scanty. Aim: To determine the effect of Aloe vera gel on clotting time, prothrombin time and plasma fibrinogen concentration in albino Wistar rats. Methods: A total of 28 adult albino Wistar rats divided ...

  17. Analytical models approximating individual processes: a validation method.

    Science.gov (United States)

    Favier, C; Degallier, N; Menkès, C E

    2010-12-01

    Upscaling population models from fine to coarse resolutions, in space, time and/or level of description, allows the derivation of fast and tractable models based on a thorough knowledge of individual processes. The validity of such approximations is generally tested only on a limited range of parameter sets. A more general validation test, over a range of parameters, is proposed; this would estimate the error induced by the approximation, using the original model's stochastic variability as a reference. This method is illustrated by three examples taken from the field of epidemics transmitted by vectors that bite in a temporally cyclical pattern, that illustrate the use of the method: to estimate if an approximation over- or under-fits the original model; to invalidate an approximation; to rank possible approximations for their qualities. As a result, the application of the validation method to this field emphasizes the need to account for the vectors' biology in epidemic prediction models and to validate these against finer scale models. Copyright © 2010 Elsevier Inc. All rights reserved.

  18. 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

  19. Case series: Bladder clot evacuation using a prostate morcellation device.

    Science.gov (United States)

    Doersch, Karen M; Navetta, Andrew F; Bird, Erin T; El Tayeb, Marawan M

    2017-07-01

    We sought to provide a technical update on the use of a prostate morcellator device (PMD) to manage organized blood clots of the bladder following laser prostatectomy. Herein, we describe our experience in using the Wolf Piranha morcellator in managing organized bladder blood clots supplemented with a retrospective chart review of the patients in whom this procedure was performed. Six patients, all male with a mean age of 75 ± 8.9 years, had organized bladder clots following either holmium laser enucleation or photoselective vaporization of the prostate managed with a PMD. Clots were recognized based on hematuria or urinary retention a median of 3.5 days following the aforementioned procedures. Initial management was attempted with more conservative measures, including a three-way Foley catheter, followed by cystoscopy with an Ellik evacuator, or a glass Tommey syringe. Morcellation times were a mean of 10.2 ± 6.15 minutes (range 2-18). This technique was able to manage clots that were an average of 173.3 ± 115.9 cc in size. The procedure was well-tolerated. No patients experienced intraoperative or morcellator-related complications. Benign prostatic hypertrophy frequently requires surgical endoscopic management and can be complicated by hematuria and bladder blood clot formation. When these clots become organized, this can lead to urinary retention and the required management, evacuation, may be difficult. The use of a Wolf Piranha PMD is a safe, well-tolerated, and effective in evacuating organized blood clots of the bladder.

  20. Shielding design method for LMFBR validation on the Phenix factor

    International Nuclear Information System (INIS)

    Cabrillat, J.C.; Crouzet, J.; Misrakis, J.; Salvatores, M.; Rado, V.; Palmiotti, G.

    1983-05-01

    Shielding design methods, developed at CEA for shielding calculations find a global validation by the means of Phenix power reactor (250 MWe) measurements. Particularly, the secondary sodium activation of pool type LMFBR such as Super Phenix (1200 MWe) which is subject to strict safety limitation is well calculated by the adapted scheme, i.e. a two dimension transport calculation of shielding coupled to a Monte-Carlo calculation of secondary sodium activation

  1. 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.

  2. Robustness study in SSNTD method validation: indoor radon quality

    International Nuclear Information System (INIS)

    Dias, D.C.S.; Silva, N.C.; Bonifácio, R.L.

    2017-01-01

    Quality control practices are indispensable to organizations aiming to reach analytical excellence. Method validation is an essential component to quality systems in laboratories, serving as a powerful tool for standardization and reliability of outcomes. This paper presents a study of robustness conducted over a SSNTD technique validation process, with the goal of developing indoor radon measurements at the highest level of quality. This quality parameter indicates how well a technique is able to provide reliable results in face of unexpected variations along the measurement. In this robustness study, based on the Youden method, 7 analytical conditions pertaining to different phases of the SSNTD technique (with focus on detector etching) were selected. Based on the ideal values for each condition as reference, extreme levels regarded as high and low were prescribed to each condition. A partial factorial design of 8 unique etching procedures was defined, where each presented their own set of high and low condition values. The Youden test provided 8 indoor radon concentration results, which allowed percentage estimations that indicate the potential influence of each analytical condition on the SSNTD technique. As expected, detector etching factors such as etching solution concentration, temperature and immersion time were identified as the most critical parameters to the technique. Detector etching is a critical step in the SSNTD method – one that must be carefully designed during validation and meticulously controlled throughout the entire process. (author)

  3. Robustness study in SSNTD method validation: indoor radon quality

    Energy Technology Data Exchange (ETDEWEB)

    Dias, D.C.S.; Silva, N.C.; Bonifácio, R.L., E-mail: danilacdias@gmail.com [Comissao Nacional de Energia Nuclear (LAPOC/CNEN), Pocos de Caldas, MG (Brazil). Laboratorio de Pocos de Caldas

    2017-07-01

    Quality control practices are indispensable to organizations aiming to reach analytical excellence. Method validation is an essential component to quality systems in laboratories, serving as a powerful tool for standardization and reliability of outcomes. This paper presents a study of robustness conducted over a SSNTD technique validation process, with the goal of developing indoor radon measurements at the highest level of quality. This quality parameter indicates how well a technique is able to provide reliable results in face of unexpected variations along the measurement. In this robustness study, based on the Youden method, 7 analytical conditions pertaining to different phases of the SSNTD technique (with focus on detector etching) were selected. Based on the ideal values for each condition as reference, extreme levels regarded as high and low were prescribed to each condition. A partial factorial design of 8 unique etching procedures was defined, where each presented their own set of high and low condition values. The Youden test provided 8 indoor radon concentration results, which allowed percentage estimations that indicate the potential influence of each analytical condition on the SSNTD technique. As expected, detector etching factors such as etching solution concentration, temperature and immersion time were identified as the most critical parameters to the technique. Detector etching is a critical step in the SSNTD method – one that must be carefully designed during validation and meticulously controlled throughout the entire process. (author)

  4. Growth of hydroxyapatite on physiologically clotted fibrin capped gold nanoparticles

    International Nuclear Information System (INIS)

    Sastry, T P; Sundaraseelan, J; Swarnalatha, K; Sobhana, S S Liji; Makheswari, M Uma; Sekar, S; Mandal, A B

    2008-01-01

    The growth of hydroxyapatite (HAp) on physiologically clotted fibrin (PCF)-gold nanoparticles is presented for the first time by employing a wet precipitation method. Fourier transform infrared (FTIR) spectroscopy confirmed the characteristic functionalities of PCF and HAp in the PCF-Au-HAp nanocomposite. Scanning electron microscopy (SEM) images have shown cuboidal nanostructures having a size in the range of 70-300 nm of HAp, whereas 2-50 nm sized particles were visualized in high-resolution transmission electron microscopy (TEM). Energy-dispersive x-ray (EDX) and x-ray diffraction (XRD) studies have confirmed the presence of HAp. These results show that gold nanoparticles with PCF acted as a matrix for the growth of HAp, and that PCF-Au-HAp nanocomposite is expected to have better osteoinductive properties

  5. Stepwise Procedure for Development and Validation of a Multipesticide Method

    Energy Technology Data Exchange (ETDEWEB)

    Ambrus, A. [Hungarian Food Safety Office, Budapest (Hungary)

    2009-07-15

    The stepwise procedure for development and the validation of so called multi-pesticide methods are described. Principles, preliminary actions, criteria for the selection of chromatographic separation, detection and performance verification of multi-pesticide methods are outlined. Also the long term repeatability and reproducibility, as well as the necessity for the documentation of laboratory work are highlighted. Appendix I hereof describes in detail the calculation of calibration parameters, whereas Appendix II focuses on the calculation of the significance of differences of concentrations obtained on two different separation columns. (author)

  6. 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. Copyright © 2012 Elsevier Inc. All rights reserved.

  7. Survey and assessment of conventional software verification and validation methods

    International Nuclear Information System (INIS)

    Miller, L.A.; Groundwater, E.; Mirsky, S.M.

    1993-04-01

    By means of a literature survey, a comprehensive set of methods was identified for the verification and validation of conventional software. The 134 methods so identified were classified according to their appropriateness for various phases of a developmental lifecycle -- requirements, design, and implementation; the last category was subdivided into two, static testing and dynamic testing methods. The methods were then characterized in terms of eight rating factors, four concerning ease-of-use of the methods and four concerning the methods' power to detect defects. Based on these factors, two measurements were developed to permit quantitative comparisons among methods, a Cost-Benefit metric and an Effectiveness Metric. The Effectiveness Metric was further refined to provide three different estimates for each method, depending on three classes of needed stringency of V ampersand V (determined by ratings of a system's complexity and required-integrity). Methods were then rank-ordered for each of the three classes in terms of their overall cost-benefits and effectiveness. The applicability was then assessed of each method for the four identified components of knowledge-based and expert systems, as well as the system as a whole

  8. Dependability validation by means of fault injection: method, implementation, application

    International Nuclear Information System (INIS)

    Arlat, Jean

    1990-01-01

    This dissertation presents theoretical and practical results concerning the use of fault injection as a means for testing fault tolerance in the framework of the experimental dependability validation of computer systems. The dissertation first presents the state-of-the-art of published work on fault injection, encompassing both hardware (fault simulation, physical fault Injection) and software (mutation testing) issues. Next, the major attributes of fault injection (faults and their activation, experimental readouts and measures, are characterized taking into account: i) the abstraction levels used to represent the system during the various phases of its development (analytical, empirical and physical models), and Il) the validation objectives (verification and evaluation). An evaluation method is subsequently proposed that combines the analytical modeling approaches (Monte Carlo Simulations, closed-form expressions. Markov chains) used for the representation of the fault occurrence process and the experimental fault Injection approaches (fault Simulation and physical injection); characterizing the error processing and fault treatment provided by the fault tolerance mechanisms. An experimental tool - MESSALINE - is then defined and presented. This tool enables physical faults to be Injected In an hardware and software prototype of the system to be validated. Finally, the application of MESSALINE for testing two fault-tolerant systems possessing very dissimilar features and the utilization of the experimental results obtained - both as design feedbacks and for dependability measures evaluation - are used to illustrate the relevance of the method. (author) [fr

  9. VALUE - Validating and Integrating Downscaling Methods for Climate Change Research

    Science.gov (United States)

    Maraun, Douglas; Widmann, Martin; Benestad, Rasmus; Kotlarski, Sven; Huth, Radan; Hertig, Elke; Wibig, Joanna; Gutierrez, Jose

    2013-04-01

    Our understanding of global climate change is mainly based on General Circulation Models (GCMs) with a relatively coarse resolution. Since climate change impacts are mainly experienced on regional scales, high-resolution climate change scenarios need to be derived from GCM simulations by downscaling. Several projects have been carried out over the last years to validate the performance of statistical and dynamical downscaling, yet several aspects have not been systematically addressed: variability on sub-daily, decadal and longer time-scales, extreme events, spatial variability and inter-variable relationships. Different downscaling approaches such as dynamical downscaling, statistical downscaling and bias correction approaches have not been systematically compared. Furthermore, collaboration between different communities, in particular regional climate modellers, statistical downscalers and statisticians has been limited. To address these gaps, the EU Cooperation in Science and Technology (COST) action VALUE (www.value-cost.eu) has been brought into life. VALUE is a research network with participants from currently 23 European countries running from 2012 to 2015. Its main aim is to systematically validate and develop downscaling methods for climate change research in order to improve regional climate change scenarios for use in climate impact studies. Inspired by the co-design idea of the international research initiative "future earth", stakeholders of climate change information have been involved in the definition of research questions to be addressed and are actively participating in the network. The key idea of VALUE is to identify the relevant weather and climate characteristics required as input for a wide range of impact models and to define an open framework to systematically validate these characteristics. Based on a range of benchmark data sets, in principle every downscaling method can be validated and compared with competing methods. The results of

  10. Validation of ultraviolet method to determine serum phosphorus level

    International Nuclear Information System (INIS)

    Garcia Borges, Lisandra; Perez Prieto, Teresa Maria; Valdes Diez, Lilliam

    2009-01-01

    Validation of a spectrophotometry method applicable in clinic labs was proposed to analytical assessment of serum phosphates using a kit UV-phosphorus of domestic production from 'Carlos J. Finlay' Biologics Production Enterprise (Havana, Cuba). Analysis method was based on phosphorus reaction to ammonium molybdenum to acid pH to creating a measurable complex to 340 nm. Specificity and precision were measured considering the method strength, linearity, accuracy and sensitivity. Analytical method was linear up to 4,8 mmol/L, precise (CV 30 .999) during clinical interest concentration interval where there were not interferences by matrix. Detection limit values were of 0.037 mmol/L and of quantification of 0.13 mmol/L both were satisfactory for product use

  11. Validity of the CT to attenuation coefficient map conversion methods

    International Nuclear Information System (INIS)

    Faghihi, R.; Ahangari Shahdehi, R.; Fazilat Moadeli, M.

    2004-01-01

    The most important commercialized methods of attenuation correction in SPECT are based on attenuation coefficient map from a transmission imaging method. The transmission imaging system can be the linear source of radioelement or a X-ray CT system. The image of transmission imaging system is not useful unless to replacement of the attenuation coefficient or CT number with the attenuation coefficient in SPECT energy. In this paper we essay to evaluate the validity and estimate the error of the most used method of this transformation. The final result shows that the methods which use a linear or multi-linear curve accept a error in their estimation. The value of mA is not important but the patient thickness is very important and it can introduce a error more than 10 percent in the final result

  12. Methods and practices for verification and validation of programmable systems

    International Nuclear Information System (INIS)

    Heimbuerger, H.; Haapanen, P.; Pulkkinen, U.

    1993-01-01

    The programmable systems deviate by their properties and behaviour from the conventional non-programmable systems in such extent, that their verification and validation for safety critical applications requires new methods and practices. The safety assessment can not be based on conventional probabilistic methods due to the difficulties in the quantification of the reliability of the software and hardware. The reliability estimate of the system must be based on qualitative arguments linked to a conservative claim limit. Due to the uncertainty of the quantitative reliability estimate other means must be used to get more assurance about the system safety. Methods and practices based on research done by VTT for STUK, are discussed in the paper as well as the methods applicable in the reliability analysis of software based safety functions. The most essential concepts and models of quantitative reliability analysis are described. The application of software models in probabilistic safety analysis (PSA) is evaluated. (author). 18 refs

  13. The Validation of NAA Method Used as Test Method in Serpong NAA Laboratory

    International Nuclear Information System (INIS)

    Rina-Mulyaningsih, Th.

    2004-01-01

    The Validation Of NAA Method Used As Test Method In Serpong NAA Laboratory. NAA Method is a non standard testing method. The testing laboratory shall validate its using method to ensure and confirm that it is suitable with application. The validation of NAA methods have been done with the parameters of accuracy, precision, repeatability and selectivity. The NIST 1573a Tomato Leaves, NIES 10C Rice flour unpolished and standard elements were used in this testing program. The result of testing with NIST 1573a showed that the elements of Na, Zn, Al and Mn are met from acceptance criteria of accuracy and precision, whereas Co is rejected. The result of testing with NIES 10C showed that Na and Zn elements are met from acceptance criteria of accuracy and precision, but Mn element is rejected. The result of selectivity test showed that the value of quantity is between 0.1-2.5 μg, depend on the elements. (author)

  14. Validation method training: nurses' experiences and ratings of work climate.

    Science.gov (United States)

    Söderlund, Mona; Norberg, Astrid; Hansebo, Görel

    2014-03-01

    Training nursing staff in communication skills can impact on the quality of care for residents with dementia and contributes to nurses' job satisfaction. Changing attitudes and practices takes time and energy and can affect the entire nursing staff, not just the nurses directly involved in a training programme. Therefore, it seems important to study nurses' experiences of a training programme and any influence of the programme on work climate among the entire nursing staff. To explore nurses' experiences of a 1-year validation method training programme conducted in a nursing home for residents with dementia and to describe ratings of work climate before and after the programme. A mixed-methods approach. Twelve nurses participated in the training and were interviewed afterwards. These individual interviews were tape-recorded and transcribed, then analysed using qualitative content analysis. The Creative Climate Questionnaire was administered before (n = 53) and after (n = 56) the programme to the entire nursing staff in the participating nursing home wards and analysed with descriptive statistics. Analysis of the interviews resulted in four categories: being under extra strain, sharing experiences, improving confidence in care situations and feeling uncertain about continuing the validation method. The results of the questionnaire on work climate showed higher mean values in the assessment after the programme had ended. The training strengthened the participating nurses in caring for residents with dementia, but posed an extra strain on them. These nurses also described an extra strain on the entire nursing staff that was not reflected in the results from the questionnaire. The work climate at the nursing home wards might have made it easier to conduct this extensive training programme. Training in the validation method could develop nurses' communication skills and improve their handling of complex care situations. © 2013 Blackwell Publishing Ltd.

  15. Utility of single-energy and dual-energy computed tomography in clot characterization: An in-vitro study.

    Science.gov (United States)

    Brinjikji, Waleed; Michalak, Gregory; Kadirvel, Ramanathan; Dai, Daying; Gilvarry, Michael; Duffy, Sharon; Kallmes, David F; McCollough, Cynthia; Leng, Shuai

    2017-06-01

    Background and purpose Because computed tomography (CT) is the most commonly used imaging modality for the evaluation of acute ischemic stroke patients, developing CT-based techniques for improving clot characterization could prove useful. The purpose of this in-vitro study was to determine which single-energy or dual-energy CT techniques provided optimum discrimination between red blood cell (RBC) and fibrin-rich clots. Materials and methods Seven clot types with varying fibrin and RBC densities were made (90% RBC, 99% RBC, 63% RBC, 36% RBC, 18% RBC and 0% RBC with high and low fibrin density) and their composition was verified histologically. Ten of each clot type were created and scanned with a second generation dual source scanner using three single (80 kV, 100 kV, 120 kV) and two dual-energy protocols (80/Sn 140 kV and 100/Sn 140 kV). A region of interest (ROI) was placed over each clot and mean attenuation was measured. Receiver operating characteristic curves were calculated at each energy level to determine the accuracy at differentiating RBC-rich clots from fibrin-rich clots. Results Clot attenuation increased with RBC content at all energy levels. Single-energy at 80 kV and 120 kV and dual-energy 80/Sn 140 kV protocols allowed for distinguishing between all clot types, with the exception of 36% RBC and 18% RBC. On receiver operating characteristic curve analysis, the 80/Sn 140 kV dual-energy protocol had the highest area under the curve for distinguishing between fibrin-rich and RBC-rich clots (area under the curve 0.99). Conclusions Dual-energy CT with 80/Sn 140 kV had the highest accuracy for differentiating RBC-rich and fibrin-rich in-vitro thrombi. Further studies are needed to study the utility of non-contrast dual-energy CT in thrombus characterization in acute ischemic stroke.

  16. Method validation and stability study of quercetin in topical emulsions

    Directory of Open Access Journals (Sweden)

    Rúbia Casagrande

    2009-01-01

    Full Text Available This study validated a high performance liquid chromatography (HPLC method for the quantitative evaluation of quercetin in topical emulsions. The method was linear within 0.05 - 200 μg/mL range with a correlation coefficient of 0.9997, and without interference in the quercetin peak. The detection and quantitation limits were 18 and 29 ng/mL, respectively. The intra- and inter-assay precisions presented R.S.D. values lower than 2%. An average of 93% and 94% of quercetin was recovered for non-ionic and anionic emulsions, respectively. The raw material and anionic emulsion, but not non-ionic emulsion, were stable in all storage conditions for one year. The method reported is a fast and reliable HPLC technique useful for quercetin determination in topical emulsions.

  17. Statistical methods for mechanistic model validation: Salt Repository Project

    International Nuclear Information System (INIS)

    Eggett, D.L.

    1988-07-01

    As part of the Department of Energy's Salt Repository Program, Pacific Northwest Laboratory (PNL) is studying the emplacement of nuclear waste containers in a salt repository. One objective of the SRP program is to develop an overall waste package component model which adequately describes such phenomena as container corrosion, waste form leaching, spent fuel degradation, etc., which are possible in the salt repository environment. The form of this model will be proposed, based on scientific principles and relevant salt repository conditions with supporting data. The model will be used to predict the future characteristics of the near field environment. This involves several different submodels such as the amount of time it takes a brine solution to contact a canister in the repository, how long it takes a canister to corrode and expose its contents to the brine, the leach rate of the contents of the canister, etc. These submodels are often tested in a laboratory and should be statistically validated (in this context, validate means to demonstrate that the model adequately describes the data) before they can be incorporated into the waste package component model. This report describes statistical methods for validating these models. 13 refs., 1 fig., 3 tabs

  18. Simulation Methods and Validation Criteria for Modeling Cardiac Ventricular Electrophysiology.

    Directory of Open Access Journals (Sweden)

    Shankarjee Krishnamoorthi

    Full Text Available We describe a sequence of methods to produce a partial differential equation model of the electrical activation of the ventricles. In our framework, we incorporate the anatomy and cardiac microstructure obtained from magnetic resonance imaging and diffusion tensor imaging of a New Zealand White rabbit, the Purkinje structure and the Purkinje-muscle junctions, and an electrophysiologically accurate model of the ventricular myocytes and tissue, which includes transmural and apex-to-base gradients of action potential characteristics. We solve the electrophysiology governing equations using the finite element method and compute both a 6-lead precordial electrocardiogram (ECG and the activation wavefronts over time. We are particularly concerned with the validation of the various methods used in our model and, in this regard, propose a series of validation criteria that we consider essential. These include producing a physiologically accurate ECG, a correct ventricular activation sequence, and the inducibility of ventricular fibrillation. Among other components, we conclude that a Purkinje geometry with a high density of Purkinje muscle junctions covering the right and left ventricular endocardial surfaces as well as transmural and apex-to-base gradients in action potential characteristics are necessary to produce ECGs and time activation plots that agree with physiological observations.

  19. Simulation Methods and Validation Criteria for Modeling Cardiac Ventricular Electrophysiology.

    Science.gov (United States)

    Krishnamoorthi, Shankarjee; Perotti, Luigi E; Borgstrom, Nils P; Ajijola, Olujimi A; Frid, Anna; Ponnaluri, Aditya V; Weiss, James N; Qu, Zhilin; Klug, William S; Ennis, Daniel B; Garfinkel, Alan

    2014-01-01

    We describe a sequence of methods to produce a partial differential equation model of the electrical activation of the ventricles. In our framework, we incorporate the anatomy and cardiac microstructure obtained from magnetic resonance imaging and diffusion tensor imaging of a New Zealand White rabbit, the Purkinje structure and the Purkinje-muscle junctions, and an electrophysiologically accurate model of the ventricular myocytes and tissue, which includes transmural and apex-to-base gradients of action potential characteristics. We solve the electrophysiology governing equations using the finite element method and compute both a 6-lead precordial electrocardiogram (ECG) and the activation wavefronts over time. We are particularly concerned with the validation of the various methods used in our model and, in this regard, propose a series of validation criteria that we consider essential. These include producing a physiologically accurate ECG, a correct ventricular activation sequence, and the inducibility of ventricular fibrillation. Among other components, we conclude that a Purkinje geometry with a high density of Purkinje muscle junctions covering the right and left ventricular endocardial surfaces as well as transmural and apex-to-base gradients in action potential characteristics are necessary to produce ECGs and time activation plots that agree with physiological observations.

  20. 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

  1. Changes in clot lysis levels of reteplase and streptokinase following continuous wave ultrasound exposure, at ultrasound intensities following attenuation from the skull bone

    Directory of Open Access Journals (Sweden)

    Roijer Anders

    2008-08-01

    Full Text Available Abstract Background Ultrasound (US has been used to enhance thrombolytic therapy in the treatment of stroke. Considerable attenuation of US intensity is however noted if US is applied over the temporal bone. The aim of this study was therefore to explore possible changes in the effect of thrombolytic drugs during low-intensity, high-frequency continuous-wave ultrasound (CW-US exposure. Methods Clots were made from fresh venous blood drawn from healthy volunteers. Each clot was made from 1.4 ml blood and left to coagulate for 1 hour in a plastic test-tube. The thrombolytic drugs used were, 3600 IU streptokinase (SK or 0.25 U reteplase (r-PA, which were mixed in 160 ml 0.9% NaCl solution. Continuous-wave US exposure was applied at a frequency of 1 MHz and intensities ranging from 0.0125 to 1.2 W/cm2. For each thrombolytic drug (n = 2, SK and r-PA and each intensity (n = 9 interventional clots (US-exposed, n = 6 were submerged in thrombolytic solution and exposed to CW-US while control clots (also submerged in thrombolytic solution, n = 6 were left unexposed to US. To evaluate the effect on clot lysis, the haemoglobin (Hb released from each clot was measured every 20 min for 1 hour (20, 40 and 60 min. The Hb content (mg released was estimated by spectrophotometry at 540 nm. The difference in effect on clot lysis was expressed as the difference in the amount of Hb released between pairs of US-exposed clots and control clots. Statistical analysis was performed using Wilcoxon's signed rank test. Results Continuous-wave ultrasound significantly decreased the effects of SK at intensities of 0.9 and 1.2 W/cm2 at all times (P 2 and at 1.2 W/cm2, following 40 min exposure at 0.3, 0.6, 0.9 and at 1.2 W/cm2, and following 60 min of exposure at 0.05 0.3, 0.6, 0.9 and at 1.2 W/cm2 (all P Conclusion Increasing intensities of CW-US exposure resulted in increased clot lysis of r-PA-treated blood clots, but decreased clot lysis of SK-treated clots.

  2. Validation study of core analysis methods for full MOX BWR

    International Nuclear Information System (INIS)

    2013-01-01

    JNES has been developing a technical database used in reviewing validation of core analysis methods of LWRs in the coming occasions: (1) confirming the core safety parameters of the initial core (one-third MOX core) through a full MOX core in Oma Nuclear Power Plant, which is under the construction, (2) licensing high-burnup MOX cores in the future and (3) reviewing topical reports on core analysis codes for safety design and evaluation. Based on the technical database, JNES will issue a guide of reviewing the core analysis methods used for safety design and evaluation of LWRs. The database will be also used for validation and improving of core analysis codes developed by JNES. JNES has progressed with the projects: (1) improving a Doppler reactivity analysis model in a Monte Carlo calculation code MVP, (2) sensitivity study of nuclear cross section date on reactivity calculation of experimental cores composed of UO 2 and MOX fuel rods, (3) analysis of isotopic composition data for UO 2 and MOX fuels and (4) the guide of reviewing the core analysis codes and others. (author)

  3. Validation study of core analysis methods for full MOX BWR

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2013-08-15

    JNES has been developing a technical database used in reviewing validation of core analysis methods of LWRs in the coming occasions: (1) confirming the core safety parameters of the initial core (one-third MOX core) through a full MOX core in Oma Nuclear Power Plant, which is under the construction, (2) licensing high-burnup MOX cores in the future and (3) reviewing topical reports on core analysis codes for safety design and evaluation. Based on the technical database, JNES will issue a guide of reviewing the core analysis methods used for safety design and evaluation of LWRs. The database will be also used for validation and improving of core analysis codes developed by JNES. JNES has progressed with the projects: (1) improving a Doppler reactivity analysis model in a Monte Carlo calculation code MVP, (2) sensitivity study of nuclear cross section date on reactivity calculation of experimental cores composed of UO{sub 2} and MOX fuel rods, (3) analysis of isotopic composition data for UO{sub 2} and MOX fuels and (4) the guide of reviewing the core analysis codes and others. (author)

  4. Validation of single-sample doubly labeled water method

    International Nuclear Information System (INIS)

    Webster, M.D.; Weathers, W.W.

    1989-01-01

    We have experimentally validated a single-sample variant of the doubly labeled water method for measuring metabolic rate and water turnover in a very small passerine bird, the verdin (Auriparus flaviceps). We measured CO 2 production using the Haldane gravimetric technique and compared these values with estimates derived from isotopic data. Doubly labeled water results based on the one-sample calculations differed from Haldane values by less than 0.5% on average (range -8.3 to 11.2%, n = 9). Water flux computed by the single-sample method differed by -1.5% on average from results for the same birds based on the standard, two-sample technique (range -13.7 to 2.0%, n = 9)

  5. Validation and further development of a novel thermal analysis method

    Energy Technology Data Exchange (ETDEWEB)

    Mathews, E.H.; Shuttleworth, A.G.; Rousseau, P.G. [Pretoria Univ. (South Africa). Dept. of Mechanical Engineering

    1994-12-31

    The design of thermal and energy efficient buildings requires inter alia the investigation of the passive performance, natural ventilation, mechanical ventilation as well as structural and evaporative cooling of the building. Only when these fail to achieve the desired thermal comfort should mechanical cooling systems be considered. Few computer programs have the ability to investigate all these comfort regulating methods at the design stage. The QUICK design program can simulate these options with the exception of mechanical cooling. In this paper, Quick`s applicability is extended to include the analysis of basic air-conditioning systems. Since the design of these systems is based on indoor loads, it was necessary to validate QUICK`s load predictions before extending it. This article addresses validation in general and proposes a procedure to establish the efficiency of a program`s load predictions. This proposed procedure is used to compare load predictions by the ASHRAE, CIBSE, CARRIER, CHEETAH, BSIMAC and QUICK methods for 46 case studies involving 36 buildings in various climatic conditions. Although significant differences in the results of the various methods were observed, it is concluded that QUICK can be used with the same confidence as the other methods. It was further shown that load prediction programs usually under-estimate the effect of building mass and therefore over-estimate the peak loads. The details for the 46 case studies are available to other researchers for further verification purposes. With the confidence gained in its load predictions, QUICK was extended to include air-conditioning system analysis. The program was then applied to different case studies. It is shown that system size and energy usage can be reduced by more than 60% by using a combination of passive and mechanical cooling systems as well as different control strategies. (author)

  6. Validation of internal dosimetry protocols based on stochastic method

    International Nuclear Information System (INIS)

    Mendes, Bruno M.; Fonseca, Telma C.F.; Almeida, Iassudara G.; Trindade, Bruno M.; Campos, Tarcisio P.R.

    2015-01-01

    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)

  7. 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)

  8. Oxcarbazepine: validation and application of an analytical method

    Directory of Open Access Journals (Sweden)

    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.

  9. Identification and characterization of milk-clotting proteases ...

    African Journals Online (AJOL)

    SAM

    2014-03-12

    Mar 12, 2014 ... Two strains of fungi were isolated and identified as Aspergillus tamarii and Penicillium pinophilum ... for milk clotting enzymes by fermentation at acid pH on culture medium containing whey ..... Rhizopus oryzae NBRC 4749.

  10. Clotting of mammalian fibrinogens by papain: A re-examination

    OpenAIRE

    Doolittle, RF

    2014-01-01

    © 2014 American Chemical Society. Papain has long been known to cause the gelation of mammalian fibrinogens. It has also been reported that papain-fibrin is insoluble in dispersing solvents like strong urea or sodium bromide solutions, similar to what is observed with thrombin-generated clots in the presence of factor XIIIa and calcium. In those old studies, both the gelation and subsequent clot stabilization were attributed to papain, although the possibility that the second step might be du...

  11. Circulating Microparticles Alter Formation, Structure, and Properties of Fibrin Clots.

    Science.gov (United States)

    Zubairova, Laily D; Nabiullina, Roza M; Nagaswami, Chandrasekaran; Zuev, Yuriy F; Mustafin, Ilshat G; Litvinov, Rustem I; Weisel, John W

    2015-12-04

    Despite the importance of circulating microparticles in haemostasis and thrombosis, there is limited evidence for potential causative effects of naturally produced cell-derived microparticles on fibrin clot formation and its properties. We studied the significance of blood microparticles for fibrin formation, structure, and susceptibility to fibrinolysis by removing them from platelet-free plasma using filtration. Clots made in platelet-free and microparticle-depleted plasma samples from the same healthy donors were analyzed in parallel. Microparticles accelerate fibrin polymerisation and support formation of more compact clots that resist internal and external fibrinolysis. These variations correlate with faster thrombin generation, suggesting thrombin-mediated kinetic effects of microparticles on fibrin formation, structure, and properties. In addition, clots formed in the presence of microparticles, unlike clots from the microparticle-depleted plasma, contain 0.1-0.5-μm size granular and CD61-positive material on fibres, suggesting that platelet-derived microparticles attach to fibrin. Therefore, the blood of healthy individuals contains functional microparticles at the levels that have a procoagulant potential. They affect the structure and stability of fibrin clots indirectly through acceleration of thrombin generation and through direct physical incorporation into the fibrin network. Both mechanisms underlie a potential role of microparticles in haemostasis and thrombosis as modulators of fibrin formation, structure, and resistance to fibrinolysis.

  12. Validation of a method for radionuclide activity optimize in SPECT

    International Nuclear Information System (INIS)

    Perez Diaz, M.; Diaz Rizo, O.; Lopez Diaz, A.; Estevez Aparicio, E.; Roque Diaz, R.

    2007-01-01

    A discriminant method for optimizing the activity administered in NM studies is validated by comparison with ROC curves. the method is tested in 21 SPECT, performed with a Cardiac phantom. Three different cold lesions (L1, L2 and L3) were placed in the myocardium-wall for each SPECT. Three activities (84 MBq, 37 MBq or 18.5 MBq) of Tc-99m diluted in water were used as background. The linear discriminant analysis was used to select the parameters that characterize image quality (Background-to-Lesion (B/L) and Signal-to-Noise (S/N) ratios). Two clusters with different image quality (p=0.021) were obtained following the selected variables. the first one involved the studies performed with 37 MBq and 84 MBq, and the second one included the studies with 18.5 MBq. the ratios B/L, B/L2 and B/L3 are the parameters capable to construct the function, with 100% of cases correctly classified into the clusters. The value of 37 MBq is the lowest tested activity for which good results for the B/Li variables were obtained,without significant differences from the results with 84 MBq (p>0.05). The result is coincident with the applied ROC-analysis. A correlation between both method of r=890 was obtained. (Author) 26 refs

  13. 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.

  14. Method for Determining Volumetric Efficiency and Its Experimental Validation

    Directory of Open Access Journals (Sweden)

    Ambrozik Andrzej

    2017-12-01

    Full Text Available Modern means of transport are basically powered by piston internal combustion engines. Increasingly rigorous demands are placed on IC engines in order to minimise the detrimental impact they have on the natural environment. That stimulates the development of research on piston internal combustion engines. The research involves experimental and theoretical investigations carried out using computer technologies. While being filled, the cylinder is considered to be an open thermodynamic system, in which non-stationary processes occur. To make calculations of thermodynamic parameters of the engine operating cycle, based on the comparison of cycles, it is necessary to know the mean constant value of cylinder pressure throughout this process. Because of the character of in-cylinder pressure pattern and difficulties in pressure experimental determination, in the present paper, a novel method for the determination of this quantity was presented. In the new approach, the iteration method was used. In the method developed for determining the volumetric efficiency, the following equations were employed: the law of conservation of the amount of substance, the first law of thermodynamics for open system, dependences for changes in the cylinder volume vs. the crankshaft rotation angle, and the state equation. The results of calculations performed with this method were validated by means of experimental investigations carried out for a selected engine at the engine test bench. A satisfactory congruence of computational and experimental results as regards determining the volumetric efficiency was obtained. The method for determining the volumetric efficiency presented in the paper can be used to investigate the processes taking place in the cylinder of an IC engine.

  15. Teaching Analytical Method Transfer through Developing and Validating Then Transferring Dissolution Testing Methods for Pharmaceuticals

    Science.gov (United States)

    Kimaru, Irene; Koether, Marina; Chichester, Kimberly; Eaton, Lafayette

    2017-01-01

    Analytical method transfer (AMT) and dissolution testing are important topics required in industry that should be taught in analytical chemistry courses. Undergraduate students in senior level analytical chemistry laboratory courses at Kennesaw State University (KSU) and St. John Fisher College (SJFC) participated in development, validation, and…

  16. A simple clot based assay for detection of procoagulant cell-derived microparticles.

    Science.gov (United States)

    Patil, Rucha; Ghosh, Kanjaksha; Shetty, Shrimati

    2016-05-01

    Cell-derived microparticles (MPs) are important biomarkers in many facets of medicine. However, the MP detection methods used till date are costly and time consuming. The main aim of this study was to standardize an in-house clot based screening method for MP detection which would not only be specific and sensitive, but also inexpensive. Four different methods of MP assessment were performed and the results correlated. Using the flow cytometry technique as the gold standard, 25 samples with normal phosphatidylserine (PS) expressing MP levels and 25 samples with elevated levels were selected, which was cross checked by the commercial STA Procoag PPL clotting time (CT) assay. A simple recalcification time and an in-house clot assay were the remaining two tests. The in-house test measures the CT after the addition of calcium chloride to MP rich plasma, following incubation with Russell viper venom and phospholipid free plasma. The CT obtained by the in-house assay significantly correlated with the results obtained by flow cytometry (R2=0.87, p<0.01). Though preliminary, the in-house assay seems to be efficient, inexpensive and promising. It could definitely be utilized routinely for procoagulant MP assessment in various clinical settings.

  17. RESULTS OF QUALITY COMPREHENSIVE EVALUATION OF DENTAL CARE FOR CHILDREN WITH BLOOD CLOTTING (PATHOLOGY

    Directory of Open Access Journals (Sweden)

    M. A. Gavrilenko

    2014-04-01

    Full Text Available Background. Treatment methods for diseases of teeth hard tissues and periodontium for children with blood clotting pathology are described in modern literature. But in practice we are faced with the problem of providing dental treatment for these children. Work of pediatric dentist is prevented by the risk of bleeding, fear of dental procedures, child’s psychoemotional tension and refusal of treatment because of bleeding. Taking into account the specificity of blood clotting pathology, surgical methods of dental treatment prevail for these children, which is evidenced by the early loss of deciduous and permanent teeth, occlusal surface disturbances, dentoalveolar anomalies, inflammatory diseases of periodontal tissues. Aim. To evaluate the level of dental care for children with the diseases of blood clotting. Materials and methods. 120 children between 2 and 18 years old with blood clotting disorders (hemophilia A, B, thrombocytopenia, thrombocytopathy were examined. Children were divided into groups: I group – 2-5 years old (40 children, II group – 6-10 years old (40 children, III group – 11-18 years old (40 children, according to the periods of tooth development, with an equal number of children in groups according to diagnoses. Clinical examination was carried out according to the standard scheme, including the analysis of complaints, anamnesis of treatment at the dentist, objective data with the use of statistical method of masticatory efficiency (according to N.I. Agapov, the level of dental care (according to P.A. Leus. Results. During clinical dental examination of children with blood clotting pathology it was found that destruction of crowns of maxillary front teeth, the first deciduous molars and the second deciduous molars, as well as their loss, prevails in the temporary occlusion. During the examination of 2-5 years old children with blood clotting pathology, loss of less than 25% of masticatory efficiency was revealed for 25

  18. Pesticide applicators questionnaire content validation: A fuzzy delphi method.

    Science.gov (United States)

    Manakandan, S K; Rosnah, I; Mohd Ridhuan, J; Priya, R

    2017-08-01

    The most crucial step in forming a set of survey questionnaire is deciding the appropriate items in a construct. Retaining irrelevant items and removing important items will certainly mislead the direction of a particular study. This article demonstrates Fuzzy Delphi method as one of the scientific analysis technique to consolidate consensus agreement within a panel of experts pertaining to each item's appropriateness. This method reduces the ambiguity, diversity, and discrepancy of the opinions among the experts hence enhances the quality of the selected items. The main purpose of this study was to obtain experts' consensus on the suitability of the preselected items on the questionnaire. The panel consists of sixteen experts from the Occupational and Environmental Health Unit of Ministry of Health, Vector-borne Disease Control Unit of Ministry of Health and Occupational and Safety Health Unit of both public and private universities. A set of questionnaires related to noise and chemical exposure were compiled based on the literature search. There was a total of six constructs with 60 items in which three constructs for knowledge, attitude, and practice of noise exposure and three constructs for knowledge, attitude, and practice of chemical exposure. The validation process replicated recent Fuzzy Delphi method that using a concept of Triangular Fuzzy Numbers and Defuzzification process. A 100% response rate was obtained from all the sixteen experts with an average Likert scoring of four to five. Post FDM analysis, the first prerequisite was fulfilled with a threshold value (d) ≤ 0.2, hence all the six constructs were accepted. For the second prerequisite, three items (21%) from noise-attitude construct and four items (40%) from chemical-practice construct had expert consensus lesser than 75%, which giving rise to about 12% from the total items in the questionnaire. The third prerequisite was used to rank the items within the constructs by calculating the average

  19. Validation of an electrophoretic method to detect albuminuria in cats.

    Science.gov (United States)

    Ferlizza, Enea; Dondi, Francesco; Andreani, Giulia; Bucci, Diego; Archer, Joy; Isani, Gloria

    2017-08-01

    Objectives The aims of this study were to validate a semi-automated high-resolution electrophoretic technique to quantify urinary albumin in healthy and diseased cats, and to evaluate its diagnostic performance in cases of proteinuria and renal diseases. Methods Urine samples were collected from 88 cats (healthy; chronic kidney disease [CKD]; lower urinary tract disease [LUTD]; non-urinary tract diseases [OTHER]). Urine samples were routinely analysed and high-resolution electrophoresis (HRE) was performed. Within-assay and between-assay variability, linearity, accuracy, recovery and the lowest detectable and quantifiable bands were calculated. Receiver operating curve (ROC) analysis was also performed. Results All coefficients of variation were HRE allowed the visualisation of a faint band of albumin and a diffused band between alpha and beta zones in healthy cats, while profiles from diseased cats were variable. Albumin (mg/dl) and urine albumin:creatinine ratio (UAC) were significantly ( P HRE is an accurate and precise method that could be used to measure albuminuria in cats. UAC was useful to correctly classify proteinuria and to discriminate between healthy and diseased cats. HRE might also provide additional information on urine proteins with a profile of all proteins (albumin and globulins) to aid clinicians in the diagnosis of diseases characterised by proteinuria.

  20. New validated method for piracetam HPLC determination in human plasma.

    Science.gov (United States)

    Curticapean, Augustin; Imre, Silvia

    2007-01-10

    The new method for HPLC determination of piracetam in human plasma was developed and validated by a new approach. The simple determination by UV detection was performed on supernatant, obtained from plasma, after proteins precipitation with perchloric acid. The chromatographic separation of piracetam under a gradient elution was achieved at room temperature with a RP-18 LiChroSpher 100 column and aqueous mobile phase containing acetonitrile and methanol. The quantitative determination of piracetam was performed at 200 nm with a lower limit of quantification LLQ=2 microg/ml. For this limit, the calculated values of the coefficient of variation and difference between mean and the nominal concentration are CV%=9.7 and bias%=0.9 for the intra-day assay, and CV%=19.1 and bias%=-7.45 for the between-days assay. For precision, the range was CV%=1.8/11.6 in the intra-day and between-days assay, and for accuracy, the range was bias%=2.3/14.9 in the intra-day and between-days assay. In addition, the stability of piracetam in different conditions was verified. Piracetam proved to be stable in plasma during 4 weeks at -20 degrees C and for 36 h at 20 degrees C in the supernatant after protein precipitation. The new proposed method was used for a bioequivalence study of two medicines containing 800 mg piracetam.

  1. An Evaluation of the Accuracy of the Subtraction Method Used for Determining Platelet Counts in Advanced Platelet-Rich Fibrin and Concentrated Growth Factor Preparations

    Directory of Open Access Journals (Sweden)

    Taisuke Watanabe

    2017-01-01

    Full Text Available Platelet concentrates should be quality-assured of purity and identity prior to clinical use. Unlike for the liquid form of platelet-rich plasma, platelet counts cannot be directly determined in solid fibrin clots and are instead calculated by subtracting the counts in other liquid or semi-clotted fractions from those in whole blood samples. Having long suspected the validity of this method, we herein examined the possible loss of platelets in the preparation process. Blood samples collected from healthy male donors were immediately centrifuged for advanced platelet-rich fibrin (A-PRF and concentrated growth factors (CGF according to recommended centrifugal protocols. Blood cells in liquid and semi-clotted fractions were directly counted. Platelets aggregated on clot surfaces were observed by scanning electron microscopy. A higher centrifugal force increased the numbers of platelets and platelet aggregates in the liquid red blood cell fraction and the semi-clotted red thrombus in the presence and absence of the anticoagulant, respectively. Nevertheless, the calculated platelet counts in A-PRF/CGF preparations were much higher than expected, rendering the currently accepted subtraction method inaccurate for determining platelet counts in fibrin clots. To ensure the quality of solid types of platelet concentrates chairside in a timely manner, a simple and accurate platelet-counting method should be developed immediately.

  2. 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;…

  3. 14-Day thawed plasma retains clot enhancing properties and inhibits tPA-induced fibrinolysis.

    Science.gov (United States)

    Huebner, Benjamin R; Moore, Ernest E; Moore, Hunter B; Shepherd-Singh, Raymond; Sauaia, Angela; Stettler, Gregory R; Nunns, Geoffrey R; Silliman, Christopher C

    2017-11-01

    Plasma-first resuscitation attenuates trauma-induced coagulopathy (TIC); however, the logistics of plasma-first resuscitation require thawed plasma (TP) be readily available due to the obligatory thawing time of fresh frozen plasma (FFP). The current standard is storage of TP for up to 5 days at 4°C, based on factor levels at outdate, for use in patients at risk for TIC, but there remains a 2.2% outdated wastage rate. However, the multitude of plasma proteins in attenuating TIC remains unknown. We hypothesize that TP retains the ability to enhance clotting and reduce tPA-induced fibrinolysis at 14-day storage. FFP was thawed and stored at 4°C at the following intervals: 14, 10, 7, 5, 3, and 1-day prior to the experiment. Healthy volunteers underwent blood draws followed by 50% dilution with TP stored at previously mentioned intervals as well as FFP, normal saline (NS), albumin, and whole blood (WB) control. Samples underwent tPA-modified (75 ng/mL) thrombelastography (TEG) with analysis of R-time, angle, maximum amplitude (MA), and LY30. TEG properties did not change significantly over the thawed storage. 14-day TP retained the ability to inhibit tPA-induced hyperfibrinolysis (median LY30% 9.6%) similar to FFP (5.6%), WB (14.6%), and superior to albumin (59.3%) and NS (58.1%). 14-day TP also retained faster clot formation (median angle, 66.2°) and superior clot strength (MA, 61.5 mm) to albumin (34.8°, 21.6 mm) and NS (41.6°, 32.2 mm). TP plasma stored for 14 days retains clot-enhancing ability and resistance to clot degradation similar to FFP. A clinical trial is needed to validate these in vitro results. Copyright © 2017 Elsevier Inc. All rights reserved.

  4. When Educational Material Is Delivered: A Mixed Methods Content Validation Study of the Information Assessment Method.

    Science.gov (United States)

    Badran, Hani; Pluye, Pierre; Grad, Roland

    2017-03-14

    The Information Assessment Method (IAM) allows clinicians to report the cognitive impact, clinical relevance, intention to use, and expected patient health benefits associated with clinical information received by email. More than 15,000 Canadian physicians and pharmacists use the IAM in continuing education programs. In addition, information providers can use IAM ratings and feedback comments from clinicians to improve their products. Our general objective was to validate the IAM questionnaire for the delivery of educational material (ecological and logical content validity). Our specific objectives were to measure the relevance and evaluate the representativeness of IAM items for assessing information received by email. A 3-part mixed methods study was conducted (convergent design). In part 1 (quantitative longitudinal study), the relevance of IAM items was measured. Participants were 5596 physician members of the Canadian Medical Association who used the IAM. A total of 234,196 ratings were collected in 2012. The relevance of IAM items with respect to their main construct was calculated using descriptive statistics (relevance ratio R). In part 2 (qualitative descriptive study), the representativeness of IAM items was evaluated. A total of 15 family physicians completed semistructured face-to-face interviews. For each construct, we evaluated the representativeness of IAM items using a deductive-inductive thematic qualitative data analysis. In part 3 (mixing quantitative and qualitative parts), results from quantitative and qualitative analyses were reviewed, juxtaposed in a table, discussed with experts, and integrated. Thus, our final results are derived from the views of users (ecological content validation) and experts (logical content validation). Of the 23 IAM items, 21 were validated for content, while 2 were removed. In part 1 (quantitative results), 21 items were deemed relevant, while 2 items were deemed not relevant (R=4.86% [N=234,196] and R=3.04% [n

  5. Tranexamic acid combined with recombinant factor VIII increases clot resistance to accelerated fibrinolysis in severe hemophilia A

    DEFF Research Database (Denmark)

    Hvas, Anne-Mette; Sørensen, Hanne Thykjær; Norengaard, Lisbeth

    2007-01-01

    examined whether the clot stability in hemophiliacs could be improved by treatment with tranexamic acid (TXA) in combination with recombinant factor VIII (rFVIII). PATIENTS/METHODS: Baseline blood samples were obtained from eight males with severe hemophilia A. Thereafter, a bolus injection of r...

  6. A method for the statistical interpretation of friction ridge skin impression evidence: Method development and validation.

    Science.gov (United States)

    Swofford, H J; Koertner, A J; Zemp, F; Ausdemore, M; Liu, A; Salyards, M J

    2018-04-03

    The forensic fingerprint community has faced increasing amounts of criticism by scientific and legal commentators, challenging the validity and reliability of fingerprint evidence due to the lack of an empirically demonstrable basis to evaluate and report the strength of the evidence in a given case. This paper presents a method, developed as a stand-alone software application, FRStat, which provides a statistical assessment of the strength of fingerprint evidence. The performance was evaluated using a variety of mated and non-mated datasets. The results show strong performance characteristics, often with values supporting specificity rates greater than 99%. This method provides fingerprint experts the capability to demonstrate the validity and reliability of fingerprint evidence in a given case and report the findings in a more transparent and standardized fashion with clearly defined criteria for conclusions and known error rate information thereby responding to concerns raised by the scientific and legal communities. Published by Elsevier B.V.

  7. Clotting mechanism in beagles irradiated by 4.5 Gy γ-rays

    International Nuclear Information System (INIS)

    Zhao Zhenhu; Wang Ning; Li Ming; Xing Shuang; Huang Haixiao; Ou Hongling; Xiong Guolin; Zhao Yanfang; Xie Ling; Wang Jinxiang; Miao Jingcheng; Zhu Nankang; Zhang Xueguang; Luo Qingliang; Cong Yuwen

    2010-01-01

    Objective: To explore the clotting mechanism in beagles irradiated by 4.5 Gy γ-rays after treatment with supportive care, or supportive care and combined cytokines. Methods: Sixteen beagles were divided into irradiation control group, Supportive care group and combined cytokines treatment group. Platelet aggregation test, thrombelastography (TEG) and the time measurement were analyzed in vitro. Results: In irradiation group and supportive care group, the platelet aggregation rates in beagles were decreased markedly and the k value of TEG was increased 7 d post-irradiation, while those indexes in combined cytokines treatment group changed little. At 14 d post-irradiation, each parameter of TEG in irradiated group changed obviously. The values of r, k, r + k and M were elevated significantly, clotting time and the maximum coagulation time of thrombus delayed, the Ma value was decreased markedly, and the maximum elasticity amplitude of thrombus was diminished. All parameters in combined cytokines treatment group were better than those in supportive care group. The thrombin time was prolonged obviously in irradiated group 14 d post-irradiation, while the thrombin time was the longest at 2-3 weeks post irradiation in supportive care group and combined cytokines treatment group (P>0.05). Conclusions: Cytokines could improve the platelet aggregation and the blood clotting functions of beagles suffering from acute radiation sickness. (authors)

  8. Real-time monitoring of human blood clotting using a lateral excited film bulk acoustic resonator

    Science.gov (United States)

    Chen, Da; Wang, Jingjng; Wang, Peng; Guo, Qiuquan; Zhang, Zhen; Ma, Jilong

    2017-04-01

    Frequent assay of hemostatic status is an essential issue for the millions of patients using anticoagulant drugs. In this paper, we presented a micro-fabricated film bulk acoustic sensor for the real-time monitoring of blood clotting and the measurement of hemostatic parameters. The device was made of an Au/ZnO/Si3N4 film stack and excited by a lateral electric field. It operated under a shear mode resonance with the frequency of 1.42 GHz and had a quality factor of 342 in human blood. During the clotting process of blood, the resonant frequency decreased along with the change of blood viscosity and showed an apparent step-ladder curve, revealing the sequential clotting stages. An important hemostatic parameter, prothrombin time, was quantitatively determined from the frequency response for different dilutions of the blood samples. The effect of a typical anticoagulant drug (heparin) on the prothrombin time was exemplarily shown. The proposed sensor displayed a good consistency and clinical comparability with the standard coagulometric methods. Thanks to the availability of direct digital signals, excellent potentials of miniaturization and integration, the proposed sensor has promising application for point-of-care coagulation technologies.

  9. Reliability and concurrent validity of an alternative method of lateral ...

    African Journals Online (AJOL)

    1 University of Northern Iowa, Division of Athletic Training, 003C Human. Performance Center, Cedar ... concurrent validity of the fingertip-to-floor distance test (FFD) ... in these protocols are spinal and extremity range of motion, pelvic control ...

  10. Alternative validation practice of an automated faulting measurement method.

    Science.gov (United States)

    2010-03-08

    A number of states have adopted profiler based systems to automatically measure faulting, : in jointed concrete pavements. However, little published work exists which documents the : validation process used for such automated faulting systems. This p...

  11. Some Important Milestones in the Field of Blood Clotting.

    Science.gov (United States)

    Doolittle, Russell F

    2016-01-01

    Several different kinds of 'milestone' in the field of blood coagulation are described from the middle decades of the 20th century. Although viewed from the standpoint of clotting per se, attention is also given to implications for innate immunity. The first milestone considered is the protracted saga of clotting dependence on vitamin K, an adventure that spanned more than five decades beginning in the 1920s. The second has to do with the discovery of a half-dozen 'new' clotting factors during the period immediately following World War II. A third pursues a narrower focus and examines the once mysterious transformation of fibrinogen into fibrin. Finally, the clinical treatment of classical hemophilia had a remarkable turning point in the 1960s as the result of simple but sensible measures. © 2015 S. Karger AG, Basel.

  12. Googling Service Boundaries for Endovascular Clot Retrieval Hub Hospitals in a Metropolitan Setting: Proof-of-Concept Study.

    Science.gov (United States)

    Phan, Thanh G; Beare, Richard; Chen, Jian; Clissold, Benjamin; Ly, John; Singhal, Shaloo; Ma, Henry; Srikanth, Velandai

    2017-05-01

    There is great interest in how endovascular clot retrieval hubs provide services to a population. We applied a computational method to objectively generate service boundaries for such endovascular clot retrieval hubs, defined by traveling time to hub. Stroke incidence data merged with population census to estimate numbers of stroke in metropolitan Melbourne, Australia. Traveling time from randomly generated addresses to 4 endovascular clot retrieval-capable hubs (Royal Melbourne Hospital [RMH], Monash Medical Center [MMC], Alfred Hospital [ALF], and Austin Hospital [AUS]) estimated using Google Map application program interface. Boundary maps generated based on traveling time at various times of day for combinations of hubs. In a 2-hub model, catchment was best distributed when RMH was paired with MMC (model 1a, RMH 1765 km 2 and MMC 1164 km 2 ) or with AUS (model 1c, RMH 1244 km 2 and AUS 1685 km 2 ), with no statistical difference between models ( P =0.20). Catchment was poorly distributed when RMH was paired with ALF (model 1b, RMH 2252 km 2 and ALF 676 km 2 ), significantly different from both models 1a and 1c (both P AUS was superior to that of RMH, MMC, and ALF in catchment distribution and travel time. The method was also successfully applied to the city of Adelaide demonstrating wider applicability. We provide proof of concept for a novel computational method to objectively designate service boundaries for endovascular clot retrieval hubs. © 2017 American Heart Association, Inc.

  13. A mixed methods inquiry into the validity of data

    Directory of Open Access Journals (Sweden)

    Vaarst Mette

    2008-07-01

    Full Text Available Abstract Background Research in herd health management solely using a quantitative approach may present major challenges to the interpretation of the results, because the humans involved may have responded to their observations based on previous experiences and own beliefs. This challenge can be met through increased awareness and dialogue between researchers and farmers or other stakeholders about the background for data collection related to management and changes in management. By integrating quantitative and qualitative research methods in a mixed methods research approach, the researchers will improve their understanding of this potential bias of the observed data and farms, which will enable them to obtain more useful results of quantitative analyses. Case description An example is used to illustrate the potentials of combining quantitative and qualitative approaches to herd health related data analyses. The example is based on two studies on bovine metritis. The first study was a quantitative observational study of risk factors for metritis in Danish dairy cows based on data from the Danish Cattle Database. The other study was a semi-structured interview study involving 20 practicing veterinarians with the aim to gain insight into veterinarians' decision making when collecting and processing data related to metritis. Discussion and Evaluation The relations between risk factors and metritis in the first project supported the findings in several other quantitative observational studies; however, the herd incidence risk was highly skewed. There may be simple practical reasons for this, e.g. underreporting and differences in the veterinarians' decision making. Additionally, the interviews in the second project identified several problems with correctness and validity of data regarding the occurrence of metritis because of differences regarding case definitions and thresholds for treatments between veterinarians. Conclusion Studies where

  14. The method validation step of biological dosimetry accreditation process

    International Nuclear Information System (INIS)

    Roy, L.; Voisin, P.A.; Guillou, A.C.; Busset, A.; Gregoire, E.; Buard, V.; Delbos, M.; Voisin, Ph.

    2006-01-01

    One of the missions of the Laboratory of Biological Dosimetry (L.D.B.) of the Institute for Radiation and Nuclear Safety (I.R.S.N.) is to assess the radiological dose after an accidental overexposure suspicion to ionising radiation, by using radio-induced changes of some biological parameters. The 'gold standard' is the yield of dicentrics observed in patients lymphocytes, and this yield is converted in dose using dose effect relationships. This method is complementary to clinical and physical dosimetry, for medical team in charge of the patients. To obtain a formal recognition of its operational activity, the laboratory decided three years ago, to require an accreditation, by following the recommendations of both 17025 General Requirements for the Competence of Testing and Calibration Laboratories and 19238 Performance criteria for service laboratories performing biological dosimetry by cyto-genetics. Diagnostics, risks analysis were realized to control the whole analysis process leading to documents writing. Purchases, personnel department, vocational training were also included in the quality system. Audits were very helpful to improve the quality system. One specificity of this technique is that it is not normalized therefore apart from quality management aspects, several technical points needed some validations. An inventory of potentially influent factors was carried out. To estimate their real effect on the yield of dicentrics, a Placket-Burman experimental design was conducted. The effect of seven parameters was tested: the BUdr (bromodeoxyuridine), PHA (phytohemagglutinin) and colcemid concentration, the culture duration, the incubator temperature, the blood volume and the medium volume. The chosen values were calculated according to the uncertainties on the way they were measured i.e. pipettes, thermometers, test tubes. None of the factors has a significant impact on the yield of dicentrics. Therefore the uncertainty linked to their use was considered as

  15. Validation of pestice multi residue analysis method on cucumber

    International Nuclear Information System (INIS)

    2011-01-01

    In this study we aimed to validate the method of multi pesticide residue analysis on cucumber. Before real sample injection, system suitability test was performed in gas chromatography (GC). For this purpose, a sensitive pesticide mixture was used for GC-NPD and estimated the performance parameters such as number of effective theoretical plates, resolution factor, asymmetry, tailing and selectivity. It was detected that the system was suitable for calibration and sample injection. Samples were fortified at the level of 0.02, 0.2, 0.8 and 1 mg/kg with mixture of dichlorvos, malathion and chloropyrifos pesticides. In the fortification step 1 4C-carbaryl was also added on homogenized analytical portions to make use of 1 4C labelled pesticides for the determining extraction efficiency. Then the basic analytical process, such as ethyl acetate extraction, filtration, evaporation and cleanup, were performed. The GPC calibration using 1 4C- carbaryl and fortification mixture (dichlorvos, malathion and chloropyrifos) showed that pesticide fraction come through the column between the 8-23 ml fractions. The recovery of 1 4C-carbaryl after the extraction and cleanup step were 92.63-111.73 % and 74.83-102.22 %, respectively. The stability of pesticides during analysis is an important factor. In this study, stability test was performed including matrix effect. Our calculation and t test results showed that above mentioned pesticides were not stabile during sample processing in our laboratory conditions and it was found that sample comminution with dry ice may improve stability. In the other part of the study, 1 4C-chloropyrifos was used to determine homogeneity of analytical portions taken from laboratory samples. Use of 1 4C labelled pesticides allows us for quick quantification analyte, even with out clean-up. The analytical results show that after sample processing with waring blender, analytical portions were homogenous. Sample processing uncertainty depending on quantity of

  16. The method validation step of biological dosimetry accreditation process

    Energy Technology Data Exchange (ETDEWEB)

    Roy, L.; Voisin, P.A.; Guillou, A.C.; Busset, A.; Gregoire, E.; Buard, V.; Delbos, M.; Voisin, Ph. [Institut de Radioprotection et de Surete Nucleaire, LDB, 92 - Fontenay aux Roses (France)

    2006-07-01

    One of the missions of the Laboratory of Biological Dosimetry (L.D.B.) of the Institute for Radiation and Nuclear Safety (I.R.S.N.) is to assess the radiological dose after an accidental overexposure suspicion to ionising radiation, by using radio-induced changes of some biological parameters. The 'gold standard' is the yield of dicentrics observed in patients lymphocytes, and this yield is converted in dose using dose effect relationships. This method is complementary to clinical and physical dosimetry, for medical team in charge of the patients. To obtain a formal recognition of its operational activity, the laboratory decided three years ago, to require an accreditation, by following the recommendations of both 17025 General Requirements for the Competence of Testing and Calibration Laboratories and 19238 Performance criteria for service laboratories performing biological dosimetry by cyto-genetics. Diagnostics, risks analysis were realized to control the whole analysis process leading to documents writing. Purchases, personnel department, vocational training were also included in the quality system. Audits were very helpful to improve the quality system. One specificity of this technique is that it is not normalized therefore apart from quality management aspects, several technical points needed some validations. An inventory of potentially influent factors was carried out. To estimate their real effect on the yield of dicentrics, a Placket-Burman experimental design was conducted. The effect of seven parameters was tested: the BUdr (bromodeoxyuridine), PHA (phytohemagglutinin) and colcemid concentration, the culture duration, the incubator temperature, the blood volume and the medium volume. The chosen values were calculated according to the uncertainties on the way they were measured i.e. pipettes, thermometers, test tubes. None of the factors has a significant impact on the yield of dicentrics. Therefore the uncertainty linked to their use was

  17. A validated RP-HPLC method for the determination of Irinotecan hydrochloride residues for cleaning validation in production area

    Directory of Open Access Journals (Sweden)

    Sunil Reddy

    2013-03-01

    Full Text Available Introduction: cleaning validation is an integral part of current good manufacturing practices in pharmaceutical industry. The main purpose of cleaning validation is to prove the effectiveness and consistency of cleaning in a given pharmaceutical production equipment to prevent cross contamination and adulteration of drug product with other active ingredient. Objective: a rapid, sensitive and specific reverse phase HPLC method was developed and validated for the quantitative determination of irinotecan hydrochloride in cleaning validation swab samples. Method: the method was validated using waters symmetry shield RP-18 (250mm x 4.6mm 5 µm column with isocratic mobile phase containing a mixture of 0.02 M potassium di-hydrogen ortho-phosphate, pH adjusted to 3.5 with ortho-phosphoric acid, methanol and acetonitrile (60:20:20 v/v/v. The flow rate of mobile phase was 1.0 mL/min with column temperature of 25°C and detection wavelength at 220nm. The sample injection volume was 100 µl. Results: the calibration curve was linear over a concentration range from 0.024 to 0.143 µg/mL with a correlation coefficient of 0.997. The intra-day and inter-day precision expressed as relative standard deviation were below 3.2%. The recoveries obtained from stainless steel, PCGI, epoxy, glass and decron cloth surfaces were more than 85% and there was no interference from the cotton swab. The detection limit (DL and quantitation limit (QL were 0.008 and 0.023 µg ml-1, respectively. Conclusion: the developed method was validated with respect to specificity, linearity, limit of detection and quantification, accuracy, precision and solution stability. The overall procedure can be used as part of a cleaning validation program in pharmaceutical manufacture of irinotecan hydrochloride.

  18. Specification and Preliminary Validation of IAT (Integrated Analysis Techniques) Methods: Executive Summary.

    Science.gov (United States)

    1985-03-01

    conceptual framwork , and preliminary validation of IAT concepts. Planned work for FY85, including more extensive validation, is also described. 20...Developments: Required Capabilities .... ......... 10 2-1 IAT Conceptual Framework - FY85 (FEO) ..... ........... 11 2-2 Recursive Nature of Decomposition...approach: 1) Identify needs & requirements for IAT. 2) Develop IAT conceptual framework. 3) Validate IAT methods. 4) Develop applications materials. To

  19. Identification and characterization of milk-clotting proteases ...

    African Journals Online (AJOL)

    Two strains of fungi were isolated and identified as Aspergillus tamarii and Penicillium pinophilum which showed good enzymatic activity on casein, 1933.33U and 1822, 21U, respectively. The search for milk clotting enzymes by fermentation at acid pH on culture medium containing whey and, after purification by molecular ...

  20. Identification and characterization of milk-clotting proteases ...

    African Journals Online (AJOL)

    SAM

    2014-03-12

    Mar 12, 2014 ... Biochem. Soc. Trans. 10:285. Hashem AM (2000). Purification and properities of a milk-clotting enzyme produced by Penicillium oxalicum. J. Bioresour. Technol. 75:219-222. Laemmli UK (1970). Cleavage of structural proteins during the assembly of the head of bacteriophage T4. Nature. 227: 680-685.

  1. Validity in Mixed Methods Research in Education: The Application of Habermas' Critical Theory

    Science.gov (United States)

    Long, Haiying

    2017-01-01

    Mixed methods approach has developed into the third methodological movement in educational research. Validity in mixed methods research as an important issue, however, has not been examined as extensively as that of quantitative and qualitative research. Additionally, the previous discussions of validity in mixed methods research focus on research…

  2. Tumour imaging by the detection of fibrin clots in tumour stroma using an anti-fibrin Fab fragment

    Science.gov (United States)

    Obonai, Toshifumi; Fuchigami, Hirobumi; Furuya, Fumiaki; Kozuka, Naoyuki; Yasunaga, Masahiro; Matsumura, Yasuhiro

    2016-01-01

    The diagnosis of early and aggressive types of cancer is important for providing effective cancer therapy. Cancer-induced fibrin clots exist only within lesions. Previously, we developed a monoclonal antibody (clone 102-10) that recognizes insoluble fibrin but not fibrinogen or soluble fibrin and confirmed that fibrin clots form continuously in various cancers. Here, we describe the development of a Fab fragment probe of clone 102-10 for tumour imaging. The distribution of 102-10 Fab was investigated in genetically engineered mice bearing pancreatic ductal adenocarcinoma (PDAC), and its effect on blood coagulation was examined. Immunohistochemical and ex vivo imaging revealed that 102-10 Fab was distributed selectively in fibrin clots in PDAC tumours 3 h after injection and that it disappeared from the body after 24 h. 102-10 Fab had no influence on blood coagulation or fibrinolysis. Tumour imaging using anti-fibrin Fab may provide a safe and effective method for the diagnosis of invasive cancers by detecting fibrin clots in tumour stroma. PMID:27009516

  3. Increased Oxidation as an Additional Mechanism Underlying Reduced Clot Permeability and Impaired Fibrinolysis in Type 2 Diabetes

    Directory of Open Access Journals (Sweden)

    Anna Lados-Krupa

    2015-01-01

    Full Text Available Aims. We sought to investigate whether enhanced oxidation contributes to unfavorable fibrin clot properties in patients with diabetes. Methods. We assessed plasma fibrin clot permeation (Ks, a measure of the pore size in fibrin networks and clot lysis time induced by recombinant tissue plasminogen activator (CLT in 163 consecutive type 2 diabetic patients (92 men and 71 women aged 65 ± 8.8 years with a mean glycated hemoglobin (HbA1c of 6.8%. We also measured oxidative stress markers, including nitrotyrosine, the soluble form of receptor for advanced glycation end products (sRAGE, 8-iso-prostaglandin F2α (8-iso-PGF2α, oxidized low-density lipoprotein (oxLDL, and advanced glycation end products (AGE. Results. There were inverse correlations between Ks and nitrotyrosine, sRAGE, 8-iso-PGF2α, and oxLDL. CLT showed a positive correlation with oxLDL and nitrotyrosine but not with other oxidation markers. All these associations remained significant for Ks after adjustment for fibrinogen, disease duration, and HbA1c (all P<0.05, while oxLDL was the only independent predictor of CLT. Conclusions. Our study shows that enhanced oxidative stress adversely affects plasma fibrin clot properties in type 2 diabetic patients, regardless of disease duration and glycemia control.

  4. Capture of lipopolysaccharide (endotoxin) by the blood clot: a comparative study.

    Science.gov (United States)

    Armstrong, Margaret T; Rickles, Frederick R; Armstrong, Peter B

    2013-01-01

    In vertebrates and arthropods, blood clotting involves the establishment of a plug of aggregated thrombocytes (the cellular clot) and an extracellular fibrillar clot formed by the polymerization of the structural protein of the clot, which is fibrin in mammals, plasma lipoprotein in crustaceans, and coagulin in the horseshoe crab, Limulus polyphemus. Both elements of the clot function to staunch bleeding. Additionally, the extracellular clot functions as an agent of the innate immune system by providing a passive anti-microbial barrier and microbial entrapment device, which functions directly at the site of wounds to the integument. Here we show that, in addition to these passive functions in immunity, the plasma lipoprotein clot of lobster, the coagulin clot of Limulus, and both the platelet thrombus and the fibrin clot of mammals (human, mouse) operate to capture lipopolysaccharide (LPS, endotoxin). The lipid A core of LPS is the principal agent of gram-negative septicemia, which is responsible for more than 100,000 human deaths annually in the United States and is similarly toxic to arthropods. Quantification using the Limulus Amebocyte Lysate (LAL) test shows that clots capture significant quantities of LPS and fluorescent-labeled LPS can be seen by microscopy to decorate the clot fibrils. Thrombi generated in the living mouse accumulate LPS in vivo. It is suggested that capture of LPS released from gram-negative bacteria entrapped by the blood clot operates to protect against the disease that might be caused by its systemic dispersal.

  5. Capture of lipopolysaccharide (endotoxin by the blood clot: a comparative study.

    Directory of Open Access Journals (Sweden)

    Margaret T Armstrong

    Full Text Available In vertebrates and arthropods, blood clotting involves the establishment of a plug of aggregated thrombocytes (the cellular clot and an extracellular fibrillar clot formed by the polymerization of the structural protein of the clot, which is fibrin in mammals, plasma lipoprotein in crustaceans, and coagulin in the horseshoe crab, Limulus polyphemus. Both elements of the clot function to staunch bleeding. Additionally, the extracellular clot functions as an agent of the innate immune system by providing a passive anti-microbial barrier and microbial entrapment device, which functions directly at the site of wounds to the integument. Here we show that, in addition to these passive functions in immunity, the plasma lipoprotein clot of lobster, the coagulin clot of Limulus, and both the platelet thrombus and the fibrin clot of mammals (human, mouse operate to capture lipopolysaccharide (LPS, endotoxin. The lipid A core of LPS is the principal agent of gram-negative septicemia, which is responsible for more than 100,000 human deaths annually in the United States and is similarly toxic to arthropods. Quantification using the Limulus Amebocyte Lysate (LAL test shows that clots capture significant quantities of LPS and fluorescent-labeled LPS can be seen by microscopy to decorate the clot fibrils. Thrombi generated in the living mouse accumulate LPS in vivo. It is suggested that capture of LPS released from gram-negative bacteria entrapped by the blood clot operates to protect against the disease that might be caused by its systemic dispersal.

  6. A French National Survey on Clotting Disorders in Mastocytosis.

    Science.gov (United States)

    Carvalhosa, Ana B; Aouba, Achille; Damaj, Gandhi; Canioni, Danielle; Brouzes, Chantal; Gyan, Emmanuel; Durupt, Stéphane; Durieu, Isabelle; Cathebras, Pascal; Costédoat-Chalumeau, Nathalie; Launay, David; Pilmis, Benoit; Barete, Stephane; Frenzel, Laurent; Lortholary, Olivier; Hermine, Olivier; Hermans, Cedric; Chandesris, Marie-Olivia

    2015-10-01

    Mastocytosis is characterized by a clonal mast cell proliferation with organ infiltration and uncontrolled degranulation. Although not characteristic and poorly explained, some patients develop clotting abnormalities. We retrospectively identified patients with established diagnosis of mastocytosis and related clotting abnormalities (clinical and/or biological) using the national French Reference Centre for Mastocytosis database. From our cohort of 14 adult patients with clotting abnormalities (median age 46 years [range 26-75]), 4 had a presentation suggestive of a primary hemostasis disorder alone (by their symptoms and/or abnormal clotting tests [PFA, von Willebrand's disease [vWD] screening]) and 10 had a laboratory impairment of secondary hemostasis. Among these, 7 had bleeds characteristic of a coagulation cascade disorder (severe/life-threatening in 5 and mild in 2 patients). Clotting abnormalities were of variable severity, typically related to intense crisis of degranulation, such as anaphylactic reactions, and/or to severe organ infiltration by mast cells. Importantly, classical hemostatic management with platelet transfusion, fresh frozen plasma, or vitamin K infusions was unsuccessful, as opposed to the use of agents inhibiting mast cell activity, particularly steroids. This illustrates the crucial role of mast cell mediators such as tryptase and heparin, which interfere both with primary (mainly via inhibition of von Willebrand factor) and secondary hemostasis. There was interestingly an unusually high number of aggressive mastocytosis (particularly mast cell leukemia) and increased mortality in the group with secondary hemostasis disorders (n = 5, 36% of the whole cohort). Mast cell degranulation and/or high tumoral burden induce both specific biologic antiaggregant and anticoagulant states with a wide clinical spectrum ranging from asymptomatic to life-threatening bleeds. Hemostatic control is achieved by mast cell inhibitors such as steroids.

  7. Adenosine diphosphate-decorated chitosan nanoparticles shorten blood clotting times, influencing the structures and varying the mechanical properties of the clots

    Directory of Open Access Journals (Sweden)

    Chung TW

    2014-03-01

    Full Text Available Tze-Wen Chung,1,3 Pei-Yi Lin,2 Shoei-Shen Wang,2 Yen-Fung Chen31Department of Biomedical Engineering, National Yang-Ming University, 2Department of Surgery, National Taiwan University Hospital, Taipei, Taiwan, Republic of China; 3Department of Chemical and Materials Engineering, National Yunlin University of Science and Technology, Yunlin, Taiwan, Republic of ChinaAbstract: Chitosan nanoparticles (NPs decorated with adenosine diphosphate (ADP (ANPs or fibrinogen (FNPs were used to fabricate hemostatic NPs that can shorten blood clotting time and prevent severe local hemorrhage. The structure and mechanical properties of the blood clot induced with ANP (clot/ANP or FNP (clot/FNP were also investigated. The NPs, ANPs, and FNPs, which had particle sizes of 245.1±14.0, 251.0±9.8, and 326.5±14.5 nm and zeta potentials of 24.1±0.5, 20.6±1.9, and 15.3±1.5 mV (n=4, respectively, were fabricated by ionic gelation and then decorated with ADP and fibrinogen. The zeta potentials and Fourier transform infrared (FTIR spectroscopy of the NPs confirmed that their surfaces were successfully coated with ADP and fibrinogen. The scanning electron microscope (SEM micrographs of the structure of the clot induced with "undecorated" chitosan NPs (clot/NP, clot/ANP, and clot/FNP (at 0.05 wt% were different, after citrated bloods had been recalcified by a calcium chloride solution containing NPs, ANPs, or FNPs. This indicated that many NPs adhered on the membrane surfaces of red blood cells, that ANPs induced many platelet aggregates, and that FNPs were incorporated into the fibrin network in the clots. Measurements of the blood clotting times (Tc of blood clot/NPs, clot/ANPs, and clot/FNPs, based on 90% of ultimate frequency shifts measured on a quartz crystal microbalance (QCM, were significantly (P<0.05 (n=4 shorter than that of a clot induced by a phosphate-buffered solution (PBS (clot/PBS (63.6%±3.1%, 48.3%±6.2%, and 63.2%±4.7%, respectively. The ∆F2

  8. Validity of the Demirjian method for dental age estimation for ...

    African Journals Online (AJOL)

    2015-02-04

    Feb 4, 2015 ... Dental age was calculated using the Demirjian's method. Chronologic age was .... in order to avoid the examiner bias at the time of collecting data. ... age using the. Demirjian method for different age groups and total sample.

  9. System Identification Methods for Aircraft Flight Control Development and Validation

    Science.gov (United States)

    1995-10-01

    System-identification methods compose a mathematical model, or series of models, : from measurements of inputs and outputs of dynamic systems. This paper : discusses the use of frequency-domain system-identification methods for the : development and ...

  10. Methods and validity of dietary assessments in four Scandinavian populations

    DEFF Research Database (Denmark)

    Bingham, S; Wiggins, H S; Englyst, H

    1982-01-01

    and duplicate collections of all food eaten, was validated by chemical analysis of the duplicates, by measuring 24-hour urine and fecal nitrogen excretion, and by comparing the constituents of the urine samples collected during the survey with similar collections 1-2 weeks later. There were good agreements...... between estimates of fat and protein intake obtained by food-table calculations of the 4-day weighed record and the chemically analyzed duplicates. Urinary plus fecal nitrogen excretion was equal to estimated nitrogen intake during the survey, and no discernable changes in urinary output occurred after...

  11. A long-term validation of the modernised DC-ARC-OES solid-sample method.

    Science.gov (United States)

    Flórián, K; Hassler, J; Förster, O

    2001-12-01

    The validation procedure based on ISO 17025 standard has been used to study and illustrate both the longterm stability of the calibration process of the DC-ARC solid sample spectrometric method and the main validation criteria of the method. In the calculation of the validation characteristics depending on the linearity(calibration), also the fulfilment of predetermining criteria such as normality and homoscedasticity was checked. In order to decide whether there are any trends in the time-variation of the analytical signal or not, also the Neumann test of trend was applied and evaluated. Finally, a comparison with similar validation data of the ETV-ICP-OES method was carried out.

  12. Content validity of methods to assess malnutrition in cancer patients: a systematic review

    NARCIS (Netherlands)

    Sealy, Martine; Nijholt, Willemke; Stuiver, M.M.; van der Berg, M.M.; Ottery, Faith D.; van der Schans, Cees; Roodenburg, Jan L N; Jager-Wittenaar, Harriët

    Content validity of methods to assess malnutrition in cancer patients: A systematic review Rationale: Inadequate operationalisation of the multidimensial concept of malnutrition may result in inadequate evaluation of nutritional status. In this review we aimed to assess content validity of methods

  13. Critical Values for Lawshe's Content Validity Ratio: Revisiting the Original Methods of Calculation

    Science.gov (United States)

    Ayre, Colin; Scally, Andrew John

    2014-01-01

    The content validity ratio originally proposed by Lawshe is widely used to quantify content validity and yet methods used to calculate the original critical values were never reported. Methods for original calculation of critical values are suggested along with tables of exact binomial probabilities.

  14. A VALIDATED STABILITY INDICATED RP-HPLC METHOD FOR DUTASTERIDE

    OpenAIRE

    D. Pavan Kumar a, b *, Naga Jhansi a, G. Srinivasa Rao b, Kirti Kumar Jain a

    2018-01-01

    ABSTRACT A Simple, Stability indicating, Isocratic, reverse phase High Performance Liquid Chromatographic (RPLC) related substance method was developed for Dutasteride in API. This method separates the impurities which are co-eluting in the pharmacopeia method. Successful separation of degradation impurities and synthetic impurities was achieved by YMC Triat phenyl column. Chromatographic was carried out on YMC Triat phenyl (150 X 4.6 mm, 3.0µm) column using 0.01M Potassium Dihydrogen Pho...

  15. Development and Validation of a Stability-Indicating LC-UV Method ...

    African Journals Online (AJOL)

    Keywords: Ketotifen, Cetirizine, Stability indicating method, Stressed conditions, Validation. Tropical ... in biological fluids [13] are also reported. Stability indicating HPLC method is reported for ketotifen where drug is ..... paracetamol, cetirizine.

  16. Validation of two ribosomal RNA removal methods for microbial metatranscriptomics

    Energy Technology Data Exchange (ETDEWEB)

    He, Shaomei; Wurtzel, Omri; Singh, Kanwar; Froula, Jeff L; Yilmaz, Suzan; Tringe, Susannah G; Wang, Zhong; Chen, Feng; Lindquist, Erika A; Sorek, Rotem; Hugenholtz, Philip

    2010-10-01

    The predominance of rRNAs in the transcriptome is a major technical challenge in sequence-based analysis of cDNAs from microbial isolates and communities. Several approaches have been applied to deplete rRNAs from (meta)transcriptomes, but no systematic investigation of potential biases introduced by any of these approaches has been reported. Here we validated the effectiveness and fidelity of the two most commonly used approaches, subtractive hybridization and exonuclease digestion, as well as combinations of these treatments, on two synthetic five-microorganism metatranscriptomes using massively parallel sequencing. We found that the effectiveness of rRNA removal was a function of community composition and RNA integrity for these treatments. Subtractive hybridization alone introduced the least bias in relative transcript abundance, whereas exonuclease and in particular combined treatments greatly compromised mRNA abundance fidelity. Illumina sequencing itself also can compromise quantitative data analysis by introducing a G+C bias between runs.

  17. Method for validating radiobiological samples using a linear accelerator

    International Nuclear Information System (INIS)

    Brengues, Muriel; Liu, David; Korn, Ronald; Zenhausern, Frederic

    2014-01-01

    There is an immediate need for rapid triage of the population in case of a large scale exposure to ionizing radiation. Knowing the dose absorbed by the body will allow clinicians to administer medical treatment for the best chance of recovery for the victim. In addition, today's radiotherapy treatment could benefit from additional information regarding the patient's sensitivity to radiation before starting the treatment. As of today, there is no system in place to respond to this demand. This paper will describe specific procedures to mimic the effects of human exposure to ionizing radiation creating the tools for optimization of administered radiation dosimetry for radiotherapy and/or to estimate the doses of radiation received accidentally during a radiation event that could pose a danger to the public. In order to obtain irradiated biological samples to study ionizing radiation absorbed by the body, we performed ex-vivo irradiation of human blood samples using the linear accelerator (LINAC). The LINAC was implemented and calibrated for irradiating human whole blood samples. To test the calibration, a 2 Gy test run was successfully performed on a tube filled with water with an accuracy of 3% in dose distribution. To validate our technique the blood samples were ex-vivo irradiated and the results were analyzed using a gene expression assay to follow the effect of the ionizing irradiation by characterizing dose responsive biomarkers from radiobiological assays. The response of 5 genes was monitored resulting in expression increase with the dose of radiation received. The blood samples treated with the LINAC can provide effective irradiated blood samples suitable for molecular profiling to validate radiobiological measurements via the gene-expression based biodosimetry tools. (orig.)

  18. Method for validating radiobiological samples using a linear accelerator.

    Science.gov (United States)

    Brengues, Muriel; Liu, David; Korn, Ronald; Zenhausern, Frederic

    2014-04-29

    There is an immediate need for rapid triage of the population in case of a large scale exposure to ionizing radiation. Knowing the dose absorbed by the body will allow clinicians to administer medical treatment for the best chance of recovery for the victim. In addition, today's radiotherapy treatment could benefit from additional information regarding the patient's sensitivity to radiation before starting the treatment. As of today, there is no system in place to respond to this demand. This paper will describe specific procedures to mimic the effects of human exposure to ionizing radiation creating the tools for optimization of administered radiation dosimetry for radiotherapy and/or to estimate the doses of radiation received accidentally during a radiation event that could pose a danger to the public. In order to obtain irradiated biological samples to study ionizing radiation absorbed by the body, we performed ex-vivo irradiation of human blood samples using the linear accelerator (LINAC). The LINAC was implemented and calibrated for irradiating human whole blood samples. To test the calibration, a 2 Gy test run was successfully performed on a tube filled with water with an accuracy of 3% in dose distribution. To validate our technique the blood samples were ex-vivo irradiated and the results were analyzed using a gene expression assay to follow the effect of the ionizing irradiation by characterizing dose responsive biomarkers from radiobiological assays. The response of 5 genes was monitored resulting in expression increase with the dose of radiation received. The blood samples treated with the LINAC can provide effective irradiated blood samples suitable for molecular profiling to validate radiobiological measurements via the gene-expression based biodosimetry tools.

  19. Effect of chitosan and coagulation factors on the wound repair phenotype of bioengineered blood clots.

    Science.gov (United States)

    Hoemann, Caroline D; Marchand, Catherine; Rivard, Georges-Etienne; El-Gabalawy, Hani; Poubelle, Patrice E

    2017-11-01

    Controlling the blood clot phenotype in a surgically prepared wound is an evolving concept in scaffold-guided tissue engineering. Here, we investigated the effect of added chitosan (80% or 95% Degree of Deacetylation, DDA) or coagulation factors (recombinant human Factor VIIa, Tissue Factor, thrombin) on inflammatory factors released by blood clots. We tested the hypothesis that 80% DDA chitosan specifically enhances leukotriene B 4 (LTB 4 ) production. Human or rabbit whole blood was combined with isotonic chitosan solutions, coagulation factors, or lipopolysaccharide, cultured in vitro at 37°C, and after 4hours the serum was assayed for LTB 4 or inflammatory factors. Only 80% DDA chitosan clots produced around 15-fold more LTB 4 over other clots including 95% DDA chitosan clots. All serum contained high levels of PDGF-BB and CXCL8. Normal clots produced very low type I cytokines compared to lipopolysaccharide clots, with even lower IL-6 and IL-12 and more CCL3/CCL4 produced by chitosan clots. Coagulation factors had no detectable effect on clot phenotype. Conclusion In blood clots from healthy individuals, 80% DDA chitosan has a unique influence of inducing more LTB 4 , a potent neutrophil chemoattractant, with similar production of PDGF-BB and CXCL8, and lower type I cytokines, compared to whole blood clots. Copyright © 2017 Elsevier B.V. All rights reserved.

  20. Development and validation of a spectroscopic method for the ...

    African Journals Online (AJOL)

    Tropical Journal of Pharmaceutical Research ... Purpose: To develop a new analytical method for the quantitative analysis of miconazole ... a simple, reliable and robust method for the characterization of a mixture of the drugs in a dosage form. ... By Country · List All Titles · Free To Read Titles This Journal is Open Access.

  1. Validated method for the detection and quantitation of synthetic ...

    African Journals Online (AJOL)

    These methods were applied to postmortem cases from the Johannesburg Forensic Pathology Services Medicolegal Laboratory (FPS-MLL) to assess the prevalence of these synthetic cannabinoids amongst the local postmortem population. Urine samples were extracted utilizing a solid phase extraction (SPE) method, ...

  2. Validation, verification and comparison: Adopting new methods in ...

    African Journals Online (AJOL)

    2005-07-03

    Jul 3, 2005 ... chemical analyses can be assumed to be homogeneously distrib- uted. When introduced ... For water microbiology this has been resolved with the publication of .... tion exercise can result in a laboratory adopting the method. If, however, the new ... For methods used for environmental sam- ples, a range of ...

  3. Testing and Validation of the Dynamic Interia Measurement Method

    Science.gov (United States)

    Chin, Alexander; Herrera, Claudia; Spivey, Natalie; Fladung, William; Cloutier, David

    2015-01-01

    This presentation describes the DIM method and how it measures the inertia properties of an object by analyzing the frequency response functions measured during a ground vibration test (GVT). The DIM method has been in development at the University of Cincinnati and has shown success on a variety of small scale test articles. The NASA AFRC version was modified for larger applications.

  4. Developing Mesoscale Model of Fibrin-Platelet Network Representing Blood Clotting =

    Science.gov (United States)

    Sun, Yueyi; Nikolov, Svetoslav; Bowie, Sam; Alexeev, Alexander; Lam, Wilbur; Myers, David

    Blood clotting disorders which prevent the body's natural ability to achieve hemostasis can lead to a variety of life threatening conditions such as, excessive bleeding, stroke, or heart attack. Treatment of these disorders is highly dependent on understanding the underlying physics behind the clotting process. Since clotting is a highly complex multi scale mechanism developing a fully atomistic model is currently not possible. We develop a mesoscale model based on dissipative particle dynamics (DPD) to gain fundamental understanding of the underlying principles controlling the clotting process. In our study, we examine experimental data on clot contraction using stacks of confocal microscopy images to estimate the crosslink density in the fibrin networks and platelet location. Using this data we reconstruct the platelet rich fibrin network and study how platelet-fibrin interactions affect clotting. Furthermore, we probe how different system parameters affect clot contraction. ANSF CAREER Award DMR-1255288.

  5. The full size validation of remanent life assessment methods

    International Nuclear Information System (INIS)

    Hepworth, J.K.; Williams, J.A.

    1988-03-01

    A range of possible life assessment techniques for the remanent life appraisal of creeping structures is available in the published literature. However, due to the safety implications, the true conservatism of such methods cannot be assessed on operating plant. Consequently, the CEGB set up a four vessel programme in the Pressure Vessel Test Facility at the Marchwood Engineering Laboratories of the CEGB to underwrite and quantify the accuracy of these methods. The application of two non-destructive methods, namely strain monitoring and hardness measurement, to the data generated during about 12,000 hours of testing is examined. The current state of development of these methods is reviewed. Finally, the future CEGB programme relating to these vessels is discussed. (author)

  6. A Validated Method for the Detection and Quantitation of Synthetic ...

    African Journals Online (AJOL)

    NICOLAAS

    A LC-HRMS (liquid chromatography coupled with high resolution mass spectrometry) method for the ... its ease of availability, from head shops (shops selling predomi- ..... cannabinoids in whole blood in plastic containers with several common ...

  7. Validation of Standing Wave Liner Impedance Measurement Method, Phase I

    Data.gov (United States)

    National Aeronautics and Space Administration — Hersh Acoustical Engineering, Inc. proposes to establish the feasibility and practicality of using the Standing Wave Method (SWM) to measure the impedance of...

  8. Validation of EIA sampling methods - bacterial and biochemical analysis

    Digital Repository Service at National Institute of Oceanography (India)

    Sheelu, G.; LokaBharathi, P.A.; Nair, S.; Raghukumar, C.; Mohandass, C.

    to temporal factors. Paired T-test between pre- and post-disturbance samples suggested that the above methods of sampling and variables like TC, protein and TOC could be used for monitoring disturbance....

  9. Development and Validation of Improved Method for Fingerprint ...

    African Journals Online (AJOL)

    Methods: The optimum high performance capillary electrophoresis (HPCE) ... organic solvent, and were analyzed using HPLC ... quantified to 200 ml with water and centrifuged at ..... for the analysis of flavonoids in selected Thai plants by.

  10. Validation of some FM-based fitness for purpose methods

    Energy Technology Data Exchange (ETDEWEB)

    Broekhoven, M J.G. [Ministry of Social Affairs, The Hague (Netherlands)

    1988-12-31

    The reliability of several FM-based fitness-for-purpose methods has been investigated on a number of objects for which accurate fracture data were available from experiments or from practice, viz. 23 wide plates, 30 mm thickness (surface and through thickness cracks, cracks at holes, with and without welds), 45 pipelines sections with cracks, pressure vessels and a T-joint. The methods applied mainly comprise ASME XI, PD 6493 and R6. This contribution reviews the results. (author). 11 refs.

  11. A mixed methods inquiry into the validity of data

    DEFF Research Database (Denmark)

    Kristensen, Erling Lundager; Nielsen, Dorthe B; Jensen, Laila N

    2008-01-01

    increased awareness and dialogue between researchers and farmers or other stakeholders about the background for data collection related to management and changes in management. By integrating quantitative and qualitative research methods in a mixed methods research approach, the researchers will improve...... greatly by adding a qualitative perspective to the quantitative approach as illustrated and discussed in this article. The combined approach requires, besides skills and interdisciplinary collaboration, also openness, reflection and scepticism from the involved scientists, but the benefits may be extended...

  12. Clot friction variation with fibrin content; implications for resistance to thrombectomy.

    Science.gov (United States)

    Gunning, Gillian M; McArdle, Kevin; Mirza, Mahmood; Duffy, Sharon; Gilvarry, Michael; Brouwer, Patrick A

    2018-01-01

    Despite significant advancements in the procedural efficacy of mechanical thrombectomy in patients with ischemic stroke in recent years, there still remains a portion of the population that does not achieve good recanalization. The reasons for this may be varied. We hypothesized that static friction between the clot and the vessel, or catheter wall might contribute to the difficulty in removing the clot. To determine if there is a relationship between clot composition and the resistance to sliding (friction) which might contribute to resistance to clot removal. As clot composition can vary significantly, we investigated five different types of clot in order to measure their respective frictional properties. To do this, a custom-made testing apparatus was created, consisting of various replaceable low-friction surfaces on which the clots could be placed. The surface was then gradually tilted until the clots began to slide; the angle at which this occurred is related to the coefficient of friction of the clots. The experiment was repeated on a bovine aortic surface in order to confirm the results. We found that fibrin-rich clots (friction than clots with a red blood cell content >20%. This result was confirmed by repeating the experiment on a bovine aortic surface as a representation of the interaction between clots and the arterial wall. The friction properties of clots were found to be related to the content ratio of fibrin to red blood cells. Future imaging techniques that could show fibrin and red blood cell content might help us to predict the 'stickiness' of a clot. Published by the BMJ Publishing Group Limited. For permission to use (where not already granted under a licence) please go to http://www.bmj.com/company/products-services/rights-and-licensing/.

  13. Validation of Alternative In Vitro Methods to Animal Testing: Concepts, Challenges, Processes and Tools.

    Science.gov (United States)

    Griesinger, Claudius; Desprez, Bertrand; Coecke, Sandra; Casey, Warren; Zuang, Valérie

    This chapter explores the concepts, processes, tools and challenges relating to the validation of alternative methods for toxicity and safety testing. In general terms, validation is the process of assessing the appropriateness and usefulness of a tool for its intended purpose. Validation is routinely used in various contexts in science, technology, the manufacturing and services sectors. It serves to assess the fitness-for-purpose of devices, systems, software up to entire methodologies. In the area of toxicity testing, validation plays an indispensable role: "alternative approaches" are increasingly replacing animal models as predictive tools and it needs to be demonstrated that these novel methods are fit for purpose. Alternative approaches include in vitro test methods, non-testing approaches such as predictive computer models up to entire testing and assessment strategies composed of method suites, data sources and decision-aiding tools. Data generated with alternative approaches are ultimately used for decision-making on public health and the protection of the environment. It is therefore essential that the underlying methods and methodologies are thoroughly characterised, assessed and transparently documented through validation studies involving impartial actors. Importantly, validation serves as a filter to ensure that only test methods able to produce data that help to address legislative requirements (e.g. EU's REACH legislation) are accepted as official testing tools and, owing to the globalisation of markets, recognised on international level (e.g. through inclusion in OECD test guidelines). Since validation creates a credible and transparent evidence base on test methods, it provides a quality stamp, supporting companies developing and marketing alternative methods and creating considerable business opportunities. Validation of alternative methods is conducted through scientific studies assessing two key hypotheses, reliability and relevance of the

  14. A guideline for the validation of likelihood ratio methods used for forensic evidence evaluation.

    Science.gov (United States)

    Meuwly, Didier; Ramos, Daniel; Haraksim, Rudolf

    2017-07-01

    This Guideline proposes a protocol for the validation of forensic evaluation methods at the source level, using the Likelihood Ratio framework as defined within the Bayes' inference model. In the context of the inference of identity of source, the Likelihood Ratio is used to evaluate the strength of the evidence for a trace specimen, e.g. a fingermark, and a reference specimen, e.g. a fingerprint, to originate from common or different sources. Some theoretical aspects of probabilities necessary for this Guideline were discussed prior to its elaboration, which started after a workshop of forensic researchers and practitioners involved in this topic. In the workshop, the following questions were addressed: "which aspects of a forensic evaluation scenario need to be validated?", "what is the role of the LR as part of a decision process?" and "how to deal with uncertainty in the LR calculation?". The questions: "what to validate?" focuses on the validation methods and criteria and "how to validate?" deals with the implementation of the validation protocol. Answers to these questions were deemed necessary with several objectives. First, concepts typical for validation standards [1], such as performance characteristics, performance metrics and validation criteria, will be adapted or applied by analogy to the LR framework. Second, a validation strategy will be defined. Third, validation methods will be described. Finally, a validation protocol and an example of validation report will be proposed, which can be applied to the forensic fields developing and validating LR methods for the evaluation of the strength of evidence at source level under the following propositions. Copyright © 2016. Published by Elsevier B.V.

  15. Flight critical system design guidelines and validation methods

    Science.gov (United States)

    Holt, H. M.; Lupton, A. O.; Holden, D. G.

    1984-01-01

    Efforts being expended at NASA-Langley to define a validation methodology, techniques for comparing advanced systems concepts, and design guidelines for characterizing fault tolerant digital avionics are described with an emphasis on the capabilities of AIRLAB, an environmentally controlled laboratory. AIRLAB has VAX 11/750 and 11/780 computers with an aggregate of 22 Mb memory and over 650 Mb storage, interconnected at 256 kbaud. An additional computer is programmed to emulate digital devices. Ongoing work is easily accessed at user stations by either chronological or key word indexing. The CARE III program aids in analyzing the capabilities of test systems to recover from faults. An additional code, the semi-Markov unreliability program (SURE) generates upper and lower reliability bounds. The AIRLAB facility is mainly dedicated to research on designs of digital flight-critical systems which must have acceptable reliability before incorporation into aircraft control systems. The digital systems would be too costly to submit to a full battery of flight tests and must be initially examined with the AIRLAB simulation capabilities.

  16. Makers of clotting medicine not entitled to liability shield.

    Science.gov (United States)

    1996-02-23

    The Indiana Court of Appeals, Second District, reversed a ruling that protected the manufacturer of a hemophilia blood clotting medicine from legal liability. A boy with hemophilia, known in court records as J.K.B. Jr., contracted HIV from the blood clotting medicine, Factor VIII. His parents sued four pharmaceutical companies, Armour Pharmaceutical Company, Cutter Laboratories, Baxter Healthcare Corporation, and Alpha Therapeutics Corporation, alleging that their products caused J.K.B. Jr.'s death. The companies convinced a Superior Court judge that they were protected under the Indiana Blood Shield Statute. The appeals court ruled that pharmaceutical companies are not included in the Blood Shield Statute. The statute was originally established to protect state-approved blood banks, hospitals, and blood storage facilities because they provide a vital public service.

  17. 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.

  18. Purification and characterization of a milk-clotting protease from ...

    African Journals Online (AJOL)

    Crude enzymatic extract obtained from five fermentations (300 g of wheat bran) was characterized by a clotting activity of 0.34 ± 0.08 UP/ml with a strength ratio of 1/1: 200. The comparative study of the summaries from 2 purification protocols showed that it is possible to recover 6% of the initial proteins with a 44.54% activity ...

  19. Likelihood ratio data to report the validation of a forensic fingerprint evaluation method

    Directory of Open Access Journals (Sweden)

    Daniel Ramos

    2017-02-01

    Full Text Available Data to which the authors refer to throughout this article are likelihood ratios (LR computed from the comparison of 5–12 minutiae fingermarks with fingerprints. These LRs data are used for the validation of a likelihood ratio (LR method in forensic evidence evaluation. These data present a necessary asset for conducting validation experiments when validating LR methods used in forensic evidence evaluation and set up validation reports. These data can be also used as a baseline for comparing the fingermark evidence in the same minutiae configuration as presented in (D. Meuwly, D. Ramos, R. Haraksim, [1], although the reader should keep in mind that different feature extraction algorithms and different AFIS systems used may produce different LRs values. Moreover, these data may serve as a reproducibility exercise, in order to train the generation of validation reports of forensic methods, according to [1]. Alongside the data, a justification and motivation for the use of methods is given. These methods calculate LRs from the fingerprint/mark data and are subject to a validation procedure. The choice of using real forensic fingerprint in the validation and simulated data in the development is described and justified. Validation criteria are set for the purpose of validation of the LR methods, which are used to calculate the LR values from the data and the validation report. For privacy and data protection reasons, the original fingerprint/mark images cannot be shared. But these images do not constitute the core data for the validation, contrarily to the LRs that are shared.

  20. The Language Teaching Methods Scale: Reliability and Validity Studies

    Science.gov (United States)

    Okmen, Burcu; Kilic, Abdurrahman

    2016-01-01

    The aim of this research is to develop a scale to determine the language teaching methods used by English teachers. The research sample consisted of 300 English teachers who taught at Duzce University and in primary schools, secondary schools and high schools in the Provincial Management of National Education in the city of Duzce in 2013-2014…

  1. A method to determine validity and reliability of activity sensors

    NARCIS (Netherlands)

    Boerema, Simone Theresa; Hermens, Hermanus J.

    2013-01-01

    METHOD Four sensors were securely fastened to a mechanical oscillator (Vibration Exciter, type 4809, Brüel & Kjær) and moved at various frequencies (6.67Hz; 13.45Hz; 19.88Hz) within the range of human physical activity. For each of the three sensor axes, the sensors were simultaneously moved for

  2. Reliability and Validity of the Research Methods Skills Assessment

    Science.gov (United States)

    Smith, Tamarah; Smith, Samantha

    2018-01-01

    The Research Methods Skills Assessment (RMSA) was created to measure psychology majors' statistics knowledge and skills. The American Psychological Association's Guidelines for the Undergraduate Major in Psychology (APA, 2007, 2013) served as a framework for development. Results from a Rasch analysis with data from n = 330 undergraduates showed…

  3. Validity of the Demirjian method for dental age estimation for ...

    African Journals Online (AJOL)

    2015-02-04

    Feb 4, 2015 ... Conclusions: It is appropriate to use the Demirjian method in southern Turkish children; however, a revision is needed in some ... Departments of Pediatric Dentistry and 1Orthodontics, Faculty of Dentistry, University of Akdeniz, Antalya, Turkey .... agenesis excluded from the study because dental anomalies.

  4. Reliability and validity of the AutoCAD software method in lumbar lordosis measurement.

    Science.gov (United States)

    Letafatkar, Amir; Amirsasan, Ramin; Abdolvahabi, Zahra; Hadadnezhad, Malihe

    2011-12-01

    The aim of this study was to determine the reliability and validity of the AutoCAD software method in lumbar lordosis measurement. Fifty healthy volunteers with a mean age of 23 ± 1.80 years were enrolled. A lumbar lateral radiograph was taken on all participants, and the lordosis was measured according to the Cobb method. Afterward, the lumbar lordosis degree was measured via AutoCAD software and flexible ruler methods. The current study is accomplished in 2 parts: intratester and intertester evaluations of reliability as well as the validity of the flexible ruler and software methods. Based on the intraclass correlation coefficient, AutoCAD's reliability and validity in measuring lumbar lordosis were 0.984 and 0.962, respectively. AutoCAD showed to be a reliable and valid method to measure lordosis. It is suggested that this method may replace those that are costly and involve health risks, such as radiography, in evaluating lumbar lordosis.

  5. 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.

  6. Comparison of Clot-based, Chromogenic, and Fluorescence Assays for Measurement of Factor VIII Inhibitors in the U.S. Hemophilia Inhibitor Research Study

    Science.gov (United States)

    Miller, Connie H.; Rice, Anne S.; Boylan, Brian; Shapiro, Amy D.; Lentz, Steven R.; Wicklund, Brian M.; Kelly, Fiona M.; Soucie, J. Michael

    2015-01-01

    Summary Background Detection and validation of inhibitors (antibodies) to hemophilia treatment products are important for clinical care, evaluation of product safety, and assessment of population trends. Methods Centralized monitoring for factor VIII (FVIII) inhibitors was conducted for patients in the Hemophilia Inhibitor Research Study using a previously reported modified Nijmegen-Bethesda clotting assay (NBA), a chromogenic Bethesda assay (CBA), and a novel fluorescence immunoassay (FLI). Results NBA and CBA were performed on 1005 specimens and FLI on 272 specimens. CBA was negative on 880/883 specimens (99.7%) with Nijmegen-Bethesda units (NBU)NBA and negative CBA, 58.1% were FLI-negative, 12.9% had evidence of lupus anticoagulant, and 35.5% had non-time-dependent inhibition. CBA and FLI were positive on 72.4% and 100% of 1.0–1.9 NBU specimens and 43.1% and 50.0% of 0.5–0.9 NBU specimens. FLI detected antibodies in 98.0% of CBA-positive and 81.6% of NBA-positive specimens (P=0.004). Among 21 new inhibitors detected by NBA, 5 (23.8%) with 0.7–1.3 NBU did not react in CBA or FLI. Among previously positive patients with 0.5–1.9 NBU, 7/25 (28%) were not CBA or FLI positive. FLI was positive on 36/169 NBU-negative specimens (21.3%). Conclusions FVIII specificity could not be demonstrated by CBA or FLI for 26% of inhibitors of 0.5–1.9 NBU; such results must be interpreted with caution. Low titer inhibitors detected in clot-based assays should always be repeated, with consideration given to evaluating their reactivity with FVIII using more specific assays. PMID:23601690

  7. Human Factors methods concerning integrated validation of nuclear power plant control rooms

    International Nuclear Information System (INIS)

    Oskarsson, Per-Anders; Johansson, Bjoern J.E.; Gonzalez, Natalia

    2010-02-01

    The frame of reference for this work was existing recommendations and instructions from the NPP area, experiences from the review of the Turbic Validation and experiences from system validations performed at the Swedish Armed Forces, e.g. concerning military control rooms and fighter pilots. These enterprises are characterized by complex systems in extreme environments, often with high risks, where human error can lead to serious consequences. A focus group has been performed with representatives responsible for Human Factors issues from all Swedish NPP:s. The questions that were discussed were, among other things, for whom an integrated validation (IV) is performed and its purpose, what should be included in an IV, the comparison with baseline measures, the design process, the role of SSM, which methods of measurement should be used, and how the methods are affected of changes in the control room. The report brings different questions to discussion concerning the validation process. Supplementary methods of measurement for integrated validation are discussed, e.g. dynamic, psychophysiological, and qualitative methods for identification of problems. Supplementary methods for statistical analysis are presented. The study points out a number of deficiencies in the validation process, e.g. the need of common guidelines for validation and design, criteria for different types of measurements, clarification of the role of SSM, and recommendations for the responsibility of external participants in the validation process. The authors propose 12 measures for taking care of the identified problems

  8. Reliability and validity of non-radiographic methods of thoracic kyphosis measurement: a systematic review.

    Science.gov (United States)

    Barrett, Eva; McCreesh, Karen; Lewis, Jeremy

    2014-02-01

    A wide array of instruments are available for non-invasive thoracic kyphosis measurement. Guidelines for selecting outcome measures for use in clinical and research practice recommend that properties such as validity and reliability are considered. This systematic review reports on the reliability and validity of non-invasive methods for measuring thoracic kyphosis. A systematic search of 11 electronic databases located studies assessing reliability and/or validity of non-invasive thoracic kyphosis measurement techniques. Two independent reviewers used a critical appraisal tool to assess the quality of retrieved studies. Data was extracted by the primary reviewer. The results were synthesized qualitatively using a level of evidence approach. 27 studies satisfied the eligibility criteria and were included in the review. The reliability, validity and both reliability and validity were investigated by sixteen, two and nine studies respectively. 17/27 studies were deemed to be of high quality. In total, 15 methods of thoracic kyphosis were evaluated in retrieved studies. All investigated methods showed high (ICC ≥ .7) to very high (ICC ≥ .9) levels of reliability. The validity of the methods ranged from low to very high. The strongest levels of evidence for reliability exists in support of the Debrunner kyphometer, Spinal Mouse and Flexicurve index, and for validity supports the arcometer and Flexicurve index. Further reliability and validity studies are required to strengthen the level of evidence for the remaining methods of measurement. This should be addressed by future research. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Validity of a Manual Soft Tissue Profile Prediction Method Following Mandibular Setback Osteotomy

    OpenAIRE

    Kolokitha, Olga-Elpis

    2007-01-01

    Objectives The aim of this study was to determine the validity of a manual cephalometric method used for predicting the post-operative soft tissue profiles of patients who underwent mandibular setback surgery and compare it to a computerized cephalometric prediction method (Dentofacial Planner). Lateral cephalograms of 18 adults with mandibular prognathism taken at the end of pre-surgical orthodontics and approximately one year after surgery were used. Methods To test the validity of the manu...

  10. TESTING METHODS FOR MECHANICALLY IMPROVED SOILS: RELIABILITY AND VALIDITY

    Directory of Open Access Journals (Sweden)

    Ana Petkovšek

    2017-10-01

    Full Text Available A possibility of in-situ mechanical improvement for reducing the liquefaction potential of silty sands was investigated by using three different techniques: Vibratory Roller Compaction, Rapid Impact Compaction (RIC and Soil Mixing. Material properties at all test sites were investigated before and after improvement with the laboratory and the in situ tests (CPT, SDMT, DPSH B, static and dynamic load plate test, geohydraulic tests. Correlation between the results obtained by different test methods gave inconclusive answers.

  11. A Virtual Upgrade Validation Method for Software-Reliant Systems

    Science.gov (United States)

    2012-06-01

    behalf of the Army Program Executive Office Aviation (PEO- AVN ). The work consists of the development of the VUV method, the subject of this report...Introduction This report is the first in a series of three reports developed by the SEI for the ASSIP and sponsored by the Army PEO AVN . This first report...Technology OQA operational quality attribute OSATE Open Source AADL Tool Environment PCI Peripheral Control Interface PEO AVN Program Executive

  12. The development and validation of control rod calculation methods

    International Nuclear Information System (INIS)

    Rowlands, J.L.; Sweet, D.W.; Franklin, B.M.

    1979-01-01

    Fission rate distributions have been measured in the zero power critical facility, ZEBRA, for a series of eight different arrays of boron carbide control rods. Diffusion theory calculations have been compared with these measurements. The normalised fission rates differ by up to about 30% in some regions, between the different arrays, and these differences are well predicted by the calculations. A development has been made to a method used to produce homogenised cross sections for lattice regions containing control rods. Calculations show that the method also reproduces the reaction rate within the rod and the fission rate dip at the surface of the rod in satisfactory agreement with the more accurate calculations which represent the fine structure of the rod. A comparison between diffusion theory and transport theory calculations of control rod reactivity worths in the CDFR shows that for the standard design method the finite mesh approximation and the difference between diffusion theory and transport theory (the transport correction) tend to cancel and result in corrections to be applied to the standard mesh diffusion theory calculations of about +- 2% or less. This result applies for mesh centred finite difference diffusion theory codes and for the arrays of natural boron carbide control rods for which the calculations were made. Improvements have also been made to the effective diffusion coefficients used in diffusion theory calculations for control rod followers and these give satisfactory agreement with transport theory calculations. (U.K.)

  13. Blood clotting and platelets: a delicate balance

    International Nuclear Information System (INIS)

    Heyns, A. du P.; Loetter, M.G.; Badenhorst, P.N.

    1988-01-01

    The Medical Research Council Blood Platelet Research Unit has studied many of the facets of platelets. The research highlights of the Unit include the following: the identification of ADPase, an enzyme found in the blood vessel wall, which breaks down adenosine diphospate (ADP) to adenosine, and which inhibits platelet aggregation; the determination of the relationship between the biochemical activity of the vessel wall with the development of atherosclerosis; the development of a method to label platelets with the compound In-111-oxine; the use of labelled platelets to study platelets in the spleen: an investigation of the life-span of platelets, which revealed how aged platelets are removed from circulation, and recently a study of methods to demonstrate in vivo activation of platelets. 1 fig

  14. Changes to the structure of blood clots formed in the presence of fine particulate matter

    International Nuclear Information System (INIS)

    Metassan, Sofian; Routledge, Michael N; Ariens, Robert A S; Scott, D Julian

    2009-01-01

    Both long-term and short-term exposure (one to two hours) to particulate matter are associated with morbidity and mortality caused by cardiovascular diseases. The underlying mechanisms leading to cardiovascular events are unclear, however, changes to blood coagulability upon exposure to ultrafine particulate matter (UFPM, the smallest of which can enter the circulation) is a plausible mechanism. Objectives: This study aims to investigate the direct effects of particulate matter on fibrin polymerization, lateral aggregation and the formation of fibrin network structure. Methods: Standard Urban Particulate Matter (PM) was suspended in Tris buffer centrifuged and filtered with <200nm filter to obtain ultrafine PM or their water-soluble components. Purified normal fibrinogen was made to clot by adding thrombin and calcium chloride in the presence of varying concentrations of PM. Permeation properties (Darcy constant [Ks]) and turbidity of clots were measured to investigate the effects on flow-rate, pore size, and fibrin polymerization. In addition, confocal microscopy was performed to study detailed clot structure. Results: Total PM increased the Ks of clots in a dose dependant manner (Ks = 4.4, 6.9 and 13.2 x 10-9 cm2 for 0, 50 and 100 |ag/ml total PM concentrations, respectively). Filtered PM also produced a significant increase in Ks at PM concentration of 17 |ag/ml. Final turbidity measurements at 20min were obtained for varying concentrations of PM. Maximum optical density (OD) for 1 mg/ml fibrinogen at 0, 50, 100 and 200 |ag/ml total PM concentrations were 0.39, 0.42, 0.45 and 0.46, respectively. The maximum OD for 0, 17, 34 and 68 |ag/ml filtered PM concentrations were 0.39, 0.42 0.47 and 0.51, respectively, suggesting an increase in fibre diameter with increasing particulate concentration. The lag phase was significantly shorter and the rate of polymerisation was significantly faster in the presence of 68 |ag/ml filtered PM. Confocal microscopy results showed

  15. Validation of the method for investigation of radiopharmaceuticals for in vitro use

    International Nuclear Information System (INIS)

    Vranjes, S; Jovanovic, M.; Orlic, M.; Lazic, E. . E-mail address of corresponding author: sanjav@vin.bg.ac.yu

    2005-01-01

    The aim of this study was to validate analytical method for determination of total radioactivity and radioactive concentration of 125 I-triiodotironin, radiopharmaceutical for in vitro use. Analytical parameters: selectivity, accuracy, linearity and range of this method were determined. Values obtained for all parameters are reasonable for analytical methods, therefore this method could be used for farther investigation. (author)

  16. Sucralfate protects blood clots from peptic digestion by gastric juice in vitro.

    Science.gov (United States)

    Nysaeter, Gunnar; Berstad, Arnold

    2006-01-01

    To test in vitro the ability of sucralfate to protect a blood clot from peptic digestion by gastric juice. Blood clots adhering to the bottom of plastic tubes were exposed to native acidic gastric juice or gastric juice to which Al-Mg antacids, sucralfate or alkali had been added. The tubes were tilted regularly at room temperature and clot digestion monitored by measuring the diameters of the clots. After 15 h, the liquids, but not the adherent clots, were poured out and the tubes refilled with native acidic gastric juice. Further clot digestion was measured, as before. Native gastric juice digested the clots completely during approximately 7 h, while in neutralized gastric juice or in gastric juice containing antacids or sucralfate no digestion was seen. In the second experiment, native gastric juice completely digested all remaining clots, except those previously exposed to sucralfate. A dose-response study indicated that gastric juice containing 3% or more of sucralfate had this long-lasting, clot-protective effect. In vitro, sucralfate adheres to and protects blood clots from digestion by gastric juice pepsin. This unique effect of sucralfate may be of clinical relevance in the treatment of bleeding peptic ulcers. Copyright 2006 S. Karger AG, Basel.

  17. Applying the Mixed Methods Instrument Development and Construct Validation Process: the Transformative Experience Questionnaire

    Science.gov (United States)

    Koskey, Kristin L. K.; Sondergeld, Toni A.; Stewart, Victoria C.; Pugh, Kevin J.

    2018-01-01

    Onwuegbuzie and colleagues proposed the Instrument Development and Construct Validation (IDCV) process as a mixed methods framework for creating and validating measures. Examples applying IDCV are lacking. We provide an illustrative case integrating the Rasch model and cognitive interviews applied to the development of the Transformative…

  18. Evaluating the Social Validity of the Early Start Denver Model: A Convergent Mixed Methods Study

    Science.gov (United States)

    Ogilvie, Emily; McCrudden, Matthew T.

    2017-01-01

    An intervention has social validity to the extent that it is socially acceptable to participants and stakeholders. This pilot convergent mixed methods study evaluated parents' perceptions of the social validity of the Early Start Denver Model (ESDM), a naturalistic behavioral intervention for children with autism. It focused on whether the parents…

  19. Rationale and methods of the European Food Consumption Validation (EFCOVAL) Project

    NARCIS (Netherlands)

    Boer, de E.J.; Slimani, N.; Boeing, H.; Feinberg, M.; Leclerq, C.; Trolle, E.; Amiano, P.; Andersen, L.F.; Freisling, H.; Geelen, A.; Harttig, U.; Huybrechts, I.; Kaic-Rak, A.; Lafay, L.; Lillegaard, I.T.L.; Ruprich, J.; Vries, de J.H.M.; Ocke, M.C.

    2011-01-01

    Background/Objectives: The overall objective of the European Food Consumption Validation (EFCOVAL) Project was to further develop and validate a trans-European food consumption method to be used for the evaluation of the intake of foods, nutrients and potentially hazardous chemicals within the

  20. Validation of Likelihood Ratio Methods Used for Forensic Evidence Evaluation: Application in Forensic Fingerprints

    NARCIS (Netherlands)

    Haraksim, Rudolf

    2014-01-01

    In this chapter the Likelihood Ratio (LR) inference model will be introduced, the theoretical aspects of probabilities will be discussed and the validation framework for LR methods used for forensic evidence evaluation will be presented. Prior to introducing the validation framework, following

  1. A Framework for Mixing Methods in Quantitative Measurement Development, Validation, and Revision: A Case Study

    Science.gov (United States)

    Luyt, Russell

    2012-01-01

    A framework for quantitative measurement development, validation, and revision that incorporates both qualitative and quantitative methods is introduced. It extends and adapts Adcock and Collier's work, and thus, facilitates understanding of quantitative measurement development, validation, and revision as an integrated and cyclical set of…

  2. Biological activity analysis of native and recombinant streptokinase using clot lysis and chromogenic substrate assay.

    Science.gov (United States)

    Mahboubi, Arash; Sadjady, Seyyed Kazem; Mirzaei Saleh Abadi, Mohammad; Azadi, Saeed; Solaimanian, Roya

    2012-01-01

    DETERMINATION OF STREPTOKINASE ACTIVITY IS USUALLY ACCOMPLISHED THROUGH TWO ASSAY METHODS: a) Clot lysis, b) Chromogenic substrate assay. In this study the biological activity of two streptokinase products, namely Streptase®, which is a native product and Heberkinasa®, which is a recombinant product, was determined against the third international reference standard using the two forementioned assay methods. The results indicated that whilst the activity of Streptase® was found to be 101 ± 4% and 97 ± 5% of the label claim with Clot lysis and Chromogenic substrate assay respectively, for Heberkinasa® the potency values obtained were 42 ± 5% and 92.5 ± 2% of the label claim respectively. To shed some light on the reason for this finding, the n-terminal sequence of the streptokinase molecules present in the two products was determined. The results showed slight differences in the amino acid sequence of the recombinant product in comparison to the native one at the amino terminus. This finding supports those of other workers who found that n-terminal sequence of the streptokinase molecule can have significant effect on the activity of this protein.

  3. Experimental Validation for Hot Stamping Process by Using Taguchi Method

    Science.gov (United States)

    Fawzi Zamri, Mohd; Lim, Syh Kai; Razlan Yusoff, Ahmad

    2016-02-01

    Due to the demand for reduction in gas emissions, energy saving and producing safer vehicles has driven the development of Ultra High Strength Steel (UHSS) material. To strengthen UHSS material such as boron steel, it needed to undergo a process of hot stamping for heating at certain temperature and time. In this paper, Taguchi method is applied to determine the appropriate parameter of thickness, heating temperature and heating time to achieve optimum strength of boron steel. The experiment is conducted by using flat square shape of hot stamping tool with tensile dog bone as a blank product. Then, the value of tensile strength and hardness is measured as response. The results showed that the lower thickness, higher heating temperature and heating time give the higher strength and hardness for the final product. In conclusion, boron steel blank are able to achieve up to 1200 MPa tensile strength and 650 HV of hardness.

  4. Validation of a spectrophotometric method for quantification of carboxyhemoglobin.

    Science.gov (United States)

    Luchini, Paulo D; Leyton, Jaime F; Strombech, Maria de Lourdes C; Ponce, Julio C; Jesus, Maria das Graças S; Leyton, Vilma

    2009-10-01

    The measurement of carboxyhemoglobin (COHb) levels in blood is a valuable procedure to confirm exposure to carbon monoxide (CO) either for forensic or occupational matters. A previously described method using spectrophotometric readings at 420 and 432 nm after reduction of oxyhemoglobin (O(2)Hb) and methemoglobin with sodium hydrosulfite solution leads to an exponential curve. This curve, used with pre-established factors, serves well for lower concentrations (1-7%) or for high concentrations (> 20%) but very rarely for both. The authors have observed that small variations on the previously described factors F1, F2, and F3, obtained from readings for 100% COHb and 100% O(2)Hb, turn into significant changes in COHb% results and propose that these factors should be determined every time COHb is measured by reading CO and O(2) saturated samples. This practice leads to an increase in accuracy and precision.

  5. VALIDATION OF THE ASSR TEST THROUGH COMPLEMENTARY AUDIOLOGYICAL METHODS

    Directory of Open Access Journals (Sweden)

    C. Mârtu

    2016-04-01

    Full Text Available Introduction: Auditory Steady State Response (ASSR is an objective method for determining the auditive threshold, applicable and necessary especially in children. The test is extremely important for recommending cochlear implant in children. The aim of the study was to compare pure tone audiometry responses and auditory steady-state thresholds. Materials and method: The study was performed on a group including both patients with normal hearing and with hearing loss. The main inclusion criteria accepted only patients with normal otomicroscopic aspect, normal tympanogram, capable to respond to pure tone audiometry, and with ear conduction thresholds between 0 and 80 dB NHL. The patients with suppurative otic processes or ear malformations were excluded. The research protocol was followed, the tests being performed in soundproofed rooms, starting with pure tone audiometry followed, after a pause, by ASSR determinations at frequencies of 0.5, 1.2 and 4 KHz. The audiological instruments were provided by a single manufacturer. ASSR was recorded at least two times for both borderline intensities, namely the one defining the auditory threshold and the first no-response intensity. The recorded responses were stored in a database and further processed in Excel. Discussion: The differences observed between pure tone audiometry and ASSR thresholds are important at 500 Hz and insignificant at the other frequencies. When approaching the PTA-ASSR relation, whatever the main characteristic between the PTA and ASSR thresholds in one ear, the profile of the lines gap maintains the same shape on the opposite ear. Conclusions: ASSR is a confident objective test, maintaining attention to low frequencies, where some differences might occur.

  6. [Use of THP-1 for allergens identification method validation].

    Science.gov (United States)

    Zhao, Xuezheng; Jia, Qiang; Zhang, Jun; Li, Xue; Zhang, Yanshu; Dai, Yufei

    2014-05-01

    Look for an in vitro test method to evaluate sensitization using THP-1 cells by the changes of the expression of cytokines to provide more reliable markers of the identification of sensitization. The monocyte-like THP-1 cells were induced and differentiated into THP-1-macrophages with PMA (0.1 microg/ml). The changes of expression of cytokines at different time points after the cells being treated with five known allergens, 2,4-dinitrochlorobenzene (DNCB), nickel sulfate (NiSO4), phenylene diamine (PPDA) potassium dichromate (K2Cr2O7) and toluene diisocyanate (TDI) and two non-allergens sodium dodecyl sulfate (SDS) and isopropanol (IPA) at various concentrations were evaluated. The IL-6 and TNF-alpha production was measured by ELISA. The secretion of IL-1beta and IL-8 was analyzed by Cytometric Bead Array (CBA). The section of the IL-6, TNF-alpha, IL-1beta and IL-8 were the highest when THP-1 cells were exposed to NiSO4, DNCB and K2Cr2O7 for 6h, PPDA and TDI for 12h. The production of IL-6 were approximately 40, 25, 20, 50 and 50 times for five kinds chemical allergens NiSO4, DNCB, K2Cr2O7, PPDA and TDI respectively at the optimum time points and the optimal concentration compared to the control group. The expression of TNF-alpha were 20, 12, 20, 8 and 5 times more than the control group respectively. IL-1beta secretion were 30, 60, 25, 30 and 45 times respectively compared to the control group. The production of IL-8 were approximately 15, 12, 15, 12 and 7 times respectively compared to the control group. Both non-allergens SDS and IPA significantly induced IL-6 secretion in a dose-dependent manner however SDS cause a higher production levels, approximately 20 times of the control. Therefore IL-6 may not be a reliable marker for identification of allergens. TNF-alpha, IL-1beta and IL-8 expressions did not change significantly after exposed to the two non-allergens. The test method using THP-1 cells by detecting the productions of cytokines (TNF-alpha, IL-1beta and

  7. Diastolic timed Vibro-Percussion at 50 Hz delivered across a chest wall sized meat barrier enhances clot dissolution and remotely administered Streptokinase effectiveness in an in-vitro model of acute coronary thrombosis

    OpenAIRE

    Hoffmann, Andrew; Gill, Harjit

    2012-01-01

    Abstract Background Low Frequency Vibro-Percussion (LFVP) assists clearance of thrombi in catheter systems and when applied to the heart and timed to diastole is known to enhance coronary flow. However LFVP on a clotted coronary like vessel given engagement over a chest wall sized barrier (to resemble non-invasive heart attack therapy) requires study. Methods One hour old clots (n=16) were dispensed within a flexible segment of Soft-Flo catheter (4 mm lumen), weighted, interfaced with Heparin...

  8. Validation needs of seismic probabilistic risk assessment (PRA) methods applied to nuclear power plants

    International Nuclear Information System (INIS)

    Kot, C.A.; Srinivasan, M.G.; Hsieh, B.J.

    1985-01-01

    An effort to validate seismic PRA methods is in progress. The work concentrates on the validation of plant response and fragility estimates through the use of test data and information from actual earthquake experience. Validation needs have been identified in the areas of soil-structure interaction, structural response and capacity, and equipment fragility. Of particular concern is the adequacy of linear methodology to predict nonlinear behavior. While many questions can be resolved through the judicious use of dynamic test data, other aspects can only be validated by means of input and response measurements during actual earthquakes. A number of past, ongoing, and planned testing programs which can provide useful validation data have been identified, and validation approaches for specific problems are being formulated

  9. Content Validity of National Post Marriage Educational Program Using Mixed Methods

    Science.gov (United States)

    MOHAJER RAHBARI, Masoumeh; SHARIATI, Mohammad; KERAMAT, Afsaneh; YUNESIAN, Masoud; ESLAMI, Mohammad; MOUSAVI, Seyed Abbas; MONTAZERI, Ali

    2015-01-01

    Background: Although the validity of content of program is mostly conducted with qualitative methods, this study used both qualitative and quantitative methods for the validation of content of post marriage training program provided for newly married couples. Content validity is a preliminary step of obtaining authorization required to install the program in country's health care system. Methods: This mixed methodological content validation study carried out in four steps with forming three expert panels. Altogether 24 expert panelists were involved in 3 qualitative and quantitative panels; 6 in the first item development one; 12 in the reduction kind, 4 of them were common with the first panel, and 10 executive experts in the last one organized to evaluate psychometric properties of CVR and CVI and Face validity of 57 educational objectives. Results: The raw data of post marriage program had been written by professional experts of Ministry of Health, using qualitative expert panel, the content was more developed by generating 3 topics and refining one topic and its respective content. In the second panel, totally six other objectives were deleted, three for being out of agreement cut of point and three on experts' consensus. The validity of all items was above 0.8 and their content validity indices (0.8–1) were completely appropriate in quantitative assessment. Conclusion: This study provided a good evidence for validation and accreditation of national post marriage program planned for newly married couples in health centers of the country in the near future. PMID:26056672

  10. Content validity across methods of malnutrition assessment in patients with cancer is limited

    NARCIS (Netherlands)

    Sealy, Martine J.; Nijholt, Willemke; Stuiver, Martijn M.; van der Berg, Marit M.; Roodenburg, Jan L. N.; Schans, van der Cees P.; Ottery, Faith D.; Jager-Wittenaar, Harriet

    Objective: To identify malnutrition assessment methods in cancer patients and assess their content validity based on internationally accepted definitions for malnutrition. Study Design and Setting: Systematic review of studies in cancer patients that operationalized malnutrition as a variable,

  11. Content validity across methods of malnutrition assessment in patients with cancer is limited

    NARCIS (Netherlands)

    Sealy, Martine; Nijholt, Willemke; Stuiver, M.M.; van der Berg, M.M.; Roodenburg, Jan; Ottery, Faith D.; van der Schans, Cees; Jager, Harriët

    2016-01-01

    Objective To identify malnutrition assessment methods in cancer patients and assess their content validity based on internationally accepted definitions for malnutrition. Study Design and Setting Systematic review of studies in cancer patients that operationalized malnutrition as a variable,

  12. Validation and application of an high-order spectral difference method for flow induced noise simulation

    KAUST Repository

    Parsani, Matteo; Ghorbaniasl, Ghader; Lacor, C.

    2011-01-01

    . The method is based on the Ffowcs WilliamsHawkings approach, which provides noise contributions for monopole, dipole and quadrupole acoustic sources. This paper will focus on the validation and assessment of this hybrid approach using different test cases

  13. An Engineering Method of Civil Jet Requirements Validation Based on Requirements Project Principle

    Science.gov (United States)

    Wang, Yue; Gao, Dan; Mao, Xuming

    2018-03-01

    A method of requirements validation is developed and defined to meet the needs of civil jet requirements validation in product development. Based on requirements project principle, this method will not affect the conventional design elements, and can effectively connect the requirements with design. It realizes the modern civil jet development concept, which is “requirement is the origin, design is the basis”. So far, the method has been successfully applied in civil jet aircraft development in China. Taking takeoff field length as an example, the validation process and the validation method of the requirements are detailed introduced in the study, with the hope of providing the experiences to other civil jet product design.

  14. Development and Validation of a RP-HPLC Method for the ...

    African Journals Online (AJOL)

    Development and Validation of a RP-HPLC Method for the Simultaneous Determination of Rifampicin and a Flavonoid Glycoside - A Novel ... range, accuracy, precision, limit of detection, limit of quantification, robustness and specificity.

  15. Probability of Detection (POD) as a statistical model for the validation of qualitative methods.

    Science.gov (United States)

    Wehling, Paul; LaBudde, Robert A; Brunelle, Sharon L; Nelson, Maria T

    2011-01-01

    A statistical model is presented for use in validation of qualitative methods. This model, termed Probability of Detection (POD), harmonizes the statistical concepts and parameters between quantitative and qualitative method validation. POD characterizes method response with respect to concentration as a continuous variable. The POD model provides a tool for graphical representation of response curves for qualitative methods. In addition, the model allows comparisons between candidate and reference methods, and provides calculations of repeatability, reproducibility, and laboratory effects from collaborative study data. Single laboratory study and collaborative study examples are given.

  16. A Generalized Pivotal Quantity Approach to Analytical Method Validation Based on Total Error.

    Science.gov (United States)

    Yang, Harry; Zhang, Jianchun

    2015-01-01

    The primary purpose of method validation is to demonstrate that the method is fit for its intended use. Traditionally, an analytical method is deemed valid if its performance characteristics such as accuracy and precision are shown to meet prespecified acceptance criteria. However, these acceptance criteria are not directly related to the method's intended purpose, which is usually a gurantee that a high percentage of the test results of future samples will be close to their true values. Alternate "fit for purpose" acceptance criteria based on the concept of total error have been increasingly used. Such criteria allow for assessing method validity, taking into account the relationship between accuracy and precision. Although several statistical test methods have been proposed in literature to test the "fit for purpose" hypothesis, the majority of the methods are not designed to protect the risk of accepting unsuitable methods, thus having the potential to cause uncontrolled consumer's risk. In this paper, we propose a test method based on generalized pivotal quantity inference. Through simulation studies, the performance of the method is compared to five existing approaches. The results show that both the new method and the method based on β-content tolerance interval with a confidence level of 90%, hereafter referred to as the β-content (0.9) method, control Type I error and thus consumer's risk, while the other existing methods do not. It is further demonstrated that the generalized pivotal quantity method is less conservative than the β-content (0.9) method when the analytical methods are biased, whereas it is more conservative when the analytical methods are unbiased. Therefore, selection of either the generalized pivotal quantity or β-content (0.9) method for an analytical method validation depends on the accuracy of the analytical method. It is also shown that the generalized pivotal quantity method has better asymptotic properties than all of the current

  17. A portable blood plasma clot micro-elastometry device based on resonant acoustic spectroscopy.

    Science.gov (United States)

    Krebs, C R; Li, Ling; Wolberg, Alisa S; Oldenburg, Amy L

    2015-07-01

    Abnormal blood clot stiffness is an important indicator of coagulation disorders arising from a variety of cardiovascular diseases and drug treatments. Here, we present a portable instrument for elastometry of microliter volume blood samples based upon the principle of resonant acoustic spectroscopy, where a sample of well-defined dimensions exhibits a fundamental longitudinal resonance mode proportional to the square root of the Young's modulus. In contrast to commercial thromboelastography, the resonant acoustic method offers improved repeatability and accuracy due to the high signal-to-noise ratio of the resonant vibration. We review the measurement principles and the design of a magnetically actuated microbead force transducer applying between 23 pN and 6.7 nN, providing a wide dynamic range of elastic moduli (3 Pa-27 kPa) appropriate for measurement of clot elastic modulus (CEM). An automated and portable device, the CEMport, is introduced and implemented using a 2 nm resolution displacement sensor with demonstrated accuracy and precision of 3% and 2%, respectively, of CEM in biogels. Importantly, the small strains (diagnostics and therapeutic monitoring.

  18. Comparing the Validity of Non-Invasive Methods in Measuring Thoracic Kyphosis and Lumbar Lordosis

    Directory of Open Access Journals (Sweden)

    Mohammad Yousefi

    2012-04-01

    Full Text Available Background: the purpose of this article is to study the validity of each of the non-invasive methods (flexible ruler, spinal mouse, and processing the image versus the one through-Ray radiation (the basic method and comparing them with each other.Materials and Methods: for evaluating the validity of each of these non-invasive methods, the thoracic Kyphosis and lumber Lordosis angle of 20 students of Birjand University (age mean and standard deviation: 26±2, weight: 72±2.5 kg, height: 169±5.5 cm through fours methods of flexible ruler, spinal mouse, and image processing and X-ray.Results: the results indicated that the validity of the methods including flexible ruler, spinal mouse, and image processing in measuring the thoracic Kyphosis and lumber Lordosis angle respectively have an adherence of 0.81, 0.87, 0.73, 0.76, 0.83, 0.89 (p>0.05. As a result, regarding the gained validity against the golden method of X-ray, it could be stated that the three mentioned non-invasive methods have adequate validity. In addition, the one-way analysis of variance test indicated that there existed a meaningful relationship between the three methods of measuring the thoracic Kyphosis and lumber Lordosis, and with respect to the Tukey’s test result, the image processing method is the most precise one.Conclusion as a result, this method could be used along with other non-invasive methods as a valid measuring method.

  19. Two Validated HPLC Methods for the Quantification of Alizarin and other Anthraquinones in Rubia tinctorum Cultivars

    NARCIS (Netherlands)

    Derksen, G.C.H.; Lelyveld, G.P.; Beek, van T.A.; Capelle, A.; Groot, de Æ.

    2004-01-01

    Direct and indirect HPLC-UV methods for the quantitative determination of anthraquinones in dried madder root have been developed, validated and compared. In the direct method, madder root was extracted twice with refluxing ethanol-water. This method allowed the determination of the two major native

  20. Determination of Modafinil in Tablet Formulation Using Three New Validated Spectrophotometric Methods

    International Nuclear Information System (INIS)

    Basniwal, P.K.; Jain, D.; Basniwal, P.K.

    2014-01-01

    In this study, three new UV spectrophotometric methods viz. linear regression equation (LRE), standard absorptivity (SA) and first order derivative (FOD) method were developed and validated for determination of modafinil in tablet form. The Beer-Lamberts law was obeyed as linear in the range of 10-50 μg/ mL and all the methods were validated for linearity, accuracy, precision and robustness. These methods were successfully applied for assay of modafinil drug content in tablets in the range of 100.20 - 100.42 %, 100.11 - 100.58 % and 100.25 - 100.34 %, respectively with acceptable standard deviation (less than two) for all the methods. The validated spectrophotometric methods may be successfully applied for assay, dissolution studies, bio-equivalence studies as well as routine analysis in pharmaceutical industries. (author)

  1. The hydraulic permeability of blood clots as a function of fibrin and platelet density.

    Science.gov (United States)

    Wufsus, A R; Macera, N E; Neeves, K B

    2013-04-16

    Interstitial fluid flow within blood clots is a biophysical mechanism that regulates clot growth and dissolution. Assuming that a clot can be modeled as a porous medium, the physical property that dictates interstitial fluid flow is the hydraulic permeability. The objective of this study was to bound the possible values of the hydraulic permeability in clots formed in vivo and present relationships that can be used to estimate clot permeability as a function of composition. A series of clots with known densities of fibrin and platelets, the two major components of a clot, were formed under static conditions. The permeability was calculated by measuring the interstitial fluid velocity through the clots at a constant pressure gradient. Fibrin gels formed with a fiber volume fraction of 0.02-0.54 had permeabilities of 1.2 × 10(-1)-1.5 × 10(-4)μm(2). Platelet-rich clots with a platelet volume fraction of 0.01-0.61 and a fibrin volume fraction of 0.03 had permeabilities over a range of 1.1 × 10(-2)-1.5 × 10(-5)μm(2). The permeability of fibrin gels and of clots with platelet volume fraction of platelet volume fraction of >0.2 were modeled as a Brinkman medium of coarse solids (platelets) embedded in a mesh of fine fibers (fibrin). Our data suggest that the permeability of clots formed in vivo can vary by up to five orders of magnitude, with pore sizes that range from 4 to 350 nm. These findings have important implications for the transport of coagulation zymogens/enzymes in the interstitial spaces during clot formation, as well as the design of fibrinolytic drug delivery strategies. Copyright © 2013 Biophysical Society. Published by Elsevier Inc. All rights reserved.

  2. Empirical Performance of Cross-Validation With Oracle Methods in a Genomics Context.

    Science.gov (United States)

    Martinez, Josue G; Carroll, Raymond J; Müller, Samuel; Sampson, Joshua N; Chatterjee, Nilanjan

    2011-11-01

    When employing model selection methods with oracle properties such as the smoothly clipped absolute deviation (SCAD) and the Adaptive Lasso, it is typical to estimate the smoothing parameter by m-fold cross-validation, for example, m = 10. In problems where the true regression function is sparse and the signals large, such cross-validation typically works well. However, in regression modeling of genomic studies involving Single Nucleotide Polymorphisms (SNP), the true regression functions, while thought to be sparse, do not have large signals. We demonstrate empirically that in such problems, the number of selected variables using SCAD and the Adaptive Lasso, with 10-fold cross-validation, is a random variable that has considerable and surprising variation. Similar remarks apply to non-oracle methods such as the Lasso. Our study strongly questions the suitability of performing only a single run of m-fold cross-validation with any oracle method, and not just the SCAD and Adaptive Lasso.

  3. 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.

  4. Validation of Cyanoacrylate Method for Collection of Stratum Corneum in Human Skin for Lipid Analysis

    DEFF Research Database (Denmark)

    Jungersted, JM; Hellgren, Lars; Drachmann, Tue

    2010-01-01

    Background and Objective: Lipids in the stratum corneum (SC) are of major importance for the skin barrier function. Many different methods have been used for the collection of SC for the analysis of SC lipids. The objective of the present study was to validate the cyanoacrylate method for the col......Background and Objective: Lipids in the stratum corneum (SC) are of major importance for the skin barrier function. Many different methods have been used for the collection of SC for the analysis of SC lipids. The objective of the present study was to validate the cyanoacrylate method...

  5. Microscale validation of 4-aminoantipyrine test method for quantifying phenolic compounds in microbial culture

    International Nuclear Information System (INIS)

    Justiz Mendoza, Ibrahin; Aguilera Rodriguez, Isabel; Perez Portuondo, Irasema

    2014-01-01

    Validation of test methods microscale is currently of great importance due to the economic and environmental advantages possessed, which constitutes a prerequisite for the performance of services and quality assurance of the results to provide customer. This paper addresses the microscale validation of 4-aminoantipyrine spectrophotometric method for the quantification of phenolic compounds in culture medium. Parameters linearity, precision, regression, accuracy, detection limits, quantification limits and robustness were evaluated, addition to the comparison test with no standardized method for determining polyphenols (Folin Ciocalteu). The results showed that both methods are feasible for determining phenols

  6. Travail et pouvoir d’agir d’Yves Clot

    Directory of Open Access Journals (Sweden)

    Jacques Leplat

    2008-11-01

    Full Text Available Yves Clot est titulaire de la Chaire de psychologie du travail du Conservatoire National des Arts et Métiers (CNAM au sein duquel il dirige l’équipe de clinique de l’activité. Cet ouvrage est le second qu’il publie dans cette collection, le premier « La fonction psychologique du travail » est paru en 1999. Entre les deux s’inscrivent un grand nombre de publications, dont beaucoup avec d’autres chercheurs, comme on pourra le constater en consultant la bibliographie de ce livre. Ce denier réun...

  7. Method development and validation of potent pyrimidine derivative by UV-VIS spectrophotometer.

    Science.gov (United States)

    Chaudhary, Anshu; Singh, Anoop; Verma, Prabhakar Kumar

    2014-12-01

    A rapid and sensitive ultraviolet-visible (UV-VIS) spectroscopic method was developed for the estimation of pyrimidine derivative 6-Bromo-3-(6-(2,6-dichlorophenyl)-2-(morpolinomethylamino) pyrimidine4-yl) -2H-chromen-2-one (BT10M) in bulk form. Pyrimidine derivative was monitored at 275 nm with UV detection, and there is no interference of diluents at 275 nm. The method was found to be linear in the range of 50 to 150 μg/ml. The accuracy and precision were determined and validated statistically. The method was validated as a guideline. The results showed that the proposed method is suitable for the accurate, precise, and rapid determination of pyrimidine derivative. Graphical Abstract Method development and validation of potent pyrimidine derivative by UV spectroscopy.

  8. [Data validation methods and discussion on Chinese materia medica resource survey].

    Science.gov (United States)

    Zhang, Yue; Ma, Wei-Feng; Zhang, Xiao-Bo; Zhu, Shou-Dong; Guo, Lan-Ping; Wang, Xing-Xing

    2013-07-01

    From the beginning of the fourth national survey of the Chinese materia medica resources, there were 22 provinces have conducted pilots. The survey teams have reported immense data, it put forward the very high request to the database system construction. In order to ensure the quality, it is necessary to check and validate the data in database system. Data validation is important methods to ensure the validity, integrity and accuracy of census data. This paper comprehensively introduce the data validation system of the fourth national survey of the Chinese materia medica resources database system, and further improve the design idea and programs of data validation. The purpose of this study is to promote the survey work smoothly.

  9. Effects of gastric bypass followed by a randomized study of physical training on markers of coagulation activation, fibrin clot properties, and fibrinolysis

    DEFF Research Database (Denmark)

    Stolberg, Charlotte Røn; Mundbjerg, Lene Hymøller; Funch-Jensen, Peter

    2018-01-01

    disease risk markers within coagulation activation, fibrin clot properties, and fibrinolysis. Setting: Bariatric center, Hospital of Southwest Jutland, Denmark. Methods: Sixty obese patients underwent RYGB and 6 months after RYGB were randomized to 26 weeks of physical training or a control group...

  10. Session-RPE Method for Training Load Monitoring: Validity, Ecological Usefulness, and Influencing Factors

    Directory of Open Access Journals (Sweden)

    Monoem Haddad

    2017-11-01

    Full Text Available Purpose: The aim of this review is to (1 retrieve all data validating the Session-rating of perceived exertion (RPE-method using various criteria, (2 highlight the rationale of this method and its ecological usefulness, and (3 describe factors that can alter RPE and users of this method should take into consideration.Method: Search engines such as SPORTDiscus, PubMed, and Google Scholar databases in the English language between 2001 and 2016 were consulted for the validity and usefulness of the session-RPE method. Studies were considered for further analysis when they used the session-RPE method proposed by Foster et al. in 2001. Participants were athletes of any gender, age, or level of competition. Studies using languages other than English were excluded in the analysis of the validity and reliability of the session-RPE method. Other studies were examined to explain the rationale of the session-RPE method and the origin of RPE.Results: A total of 950 studies cited the Foster et al. study that proposed the session RPE-method. 36 studies have examined the validity and reliability of this proposed method using the modified CR-10.Conclusion: These studies confirmed the validity and good reliability and internal consistency of session-RPE method in several sports and physical activities with men and women of different age categories (children, adolescents, and adults among various expertise levels. This method could be used as “standing alone” method for training load (TL monitoring purposes though some recommend to combine it with other physiological parameters as heart rate.

  11. Fibrinolytic Activity and Dose-Dependent Effect of Incubating Human Blood Clots in Caffeic Acid Phenethyl Ester: In Vitro Assays

    Directory of Open Access Journals (Sweden)

    Abuzar Elnager

    2015-01-01

    Full Text Available Background. Caffeic acid phenethyl ester (CAPE has been reported to possess time-dependent fibrinolytic activity by in vitro assay. This study is aimed at investigating fibrinolytic dose-dependent activity of CAPE using in vitro assays. Methods. Standardized human whole blood (WB clots were incubated in either blank controls or different concentrations of CAPE (3.75, 7.50, 15.00, 22.50, and 30.00 mM. After 3 hours, D-dimer (DD levels and WB clot weights were measured for each concentration. Thromboelastography (TEG parameters were recorded following CAPE incubation, and fibrin morphology was examined under a confocal microscope. Results. Overall, mean DD (μg/mL levels were significantly different across samples incubated with different CAPE concentrations, and the median pre- and postincubation WB clot weights (grams were significantly decreased for each CAPE concentration. Fibrin removal was observed microscopically and indicated dose-dependent effects. Based on the TEG test, the Ly30 fibrinolytic parameter was significantly different between samples incubated with two different CAPE concentrations (15.0 and 22.50 mM. The 50% effective dose (ED50 of CAPE (based on DD was 1.99 mg/mL. Conclusions. This study suggests that CAPE possesses fibrinolytic activity following in vitro incubation and that it has dose-dependent activities. Therefore, further investigation into CAPE as a potential alternative thrombolytic agent should be conducted.

  12. Development and validation of a dissolution method using HPLC for diclofenac potassium in oral suspension

    Directory of Open Access Journals (Sweden)

    Alexandre Machado Rubim

    2014-04-01

    Full Text Available The present study describes the development and validation of an in vitro dissolution method for evaluation to release diclofenac potassium in oral suspension. The dissolution test was developed and validated according to international guidelines. Parameters like linearity, specificity, precision and accuracy were evaluated, as well as the influence of rotation speed and surfactant concentration on the medium. After selecting the best conditions, the method was validated using apparatus 2 (paddle, 50-rpm rotation speed, 900 mL of water with 0.3% sodium lauryl sulfate (SLS as dissolution medium at 37.0 ± 0.5°C. Samples were analyzed using the HPLC-UV (PDA method. The results obtained were satisfactory for the parameters evaluated. The method developed may be useful in routine quality control for pharmaceutical industries that produce oral suspensions containing diclofenac potassium.

  13. Validation of innovative technologies and strategies for regulatory safety assessment methods: challenges and opportunities.

    Science.gov (United States)

    Stokes, William S; Wind, Marilyn

    2010-01-01

    Advances in science and innovative technologies are providing new opportunities to develop test methods and strategies that may improve safety assessments and reduce animal use for safety testing. These include high throughput screening and other approaches that can rapidly measure or predict various molecular, genetic, and cellular perturbations caused by test substances. Integrated testing and decision strategies that consider multiple types of information and data are also being developed. Prior to their use for regulatory decision-making, new methods and strategies must undergo appropriate validation studies to determine the extent that their use can provide equivalent or improved protection compared to existing methods and to determine the extent that reproducible results can be obtained in different laboratories. Comprehensive and optimal validation study designs are expected to expedite the validation and regulatory acceptance of new test methods and strategies that will support improved safety assessments and reduced animal use for regulatory testing.

  14. ReSOLV: Applying Cryptocurrency Blockchain Methods to Enable Global Cross-Platform Software License Validation

    Directory of Open Access Journals (Sweden)

    Alan Litchfield

    2018-05-01

    Full Text Available This paper presents a method for a decentralised peer-to-peer software license validation system using cryptocurrency blockchain technology to ameliorate software piracy, and to provide a mechanism for software developers to protect copyrighted works. Protecting software copyright has been an issue since the late 1970s and software license validation has been a primary method employed in an attempt to minimise software piracy and protect software copyright. The method described creates an ecosystem in which the rights and privileges of participants are observed.

  15. Increased efficacy for in-house validation of real-time PCR GMO detection methods.

    Science.gov (United States)

    Scholtens, I M J; Kok, E J; Hougs, L; Molenaar, B; Thissen, J T N M; van der Voet, H

    2010-03-01

    To improve the efficacy of the in-house validation of GMO detection methods (DNA isolation and real-time PCR, polymerase chain reaction), a study was performed to gain insight in the contribution of the different steps of the GMO detection method to the repeatability and in-house reproducibility. In the present study, 19 methods for (GM) soy, maize canola and potato were validated in-house of which 14 on the basis of an 8-day validation scheme using eight different samples and five on the basis of a more concise validation protocol. In this way, data was obtained with respect to the detection limit, accuracy and precision. Also, decision limits were calculated for declaring non-conformance (>0.9%) with 95% reliability. In order to estimate the contribution of the different steps in the GMO analysis to the total variation variance components were estimated using REML (residual maximum likelihood method). From these components, relative standard deviations for repeatability and reproducibility (RSD(r) and RSD(R)) were calculated. The results showed that not only the PCR reaction but also the factors 'DNA isolation' and 'PCR day' are important factors for the total variance and should therefore be included in the in-house validation. It is proposed to use a statistical model to estimate these factors from a large dataset of initial validations so that for similar GMO methods in the future, only the PCR step needs to be validated. The resulting data are discussed in the light of agreed European criteria for qualified GMO detection methods.

  16. The Effect of a Simulated Commercial Flight Environment with Hypoxia and Low Humidity on Clotting, Platelet, and Endothelial Function in Participants with Type 2 Diabetes – A Cross-over Study

    Directory of Open Access Journals (Sweden)

    Judit Konya

    2018-02-01

    Full Text Available AimsTo determine if clotting, platelet, and endothelial function were affected by simulated short-haul commercial air flight conditions (SF in participants with type 2 diabetes (T2DM compared to controls.Methods10 participants with T2DM (7 females, 3 males and 10 controls (3 females, 7 males completed the study. Participants were randomized to either spend 2 h in an environmental chamber at sea level conditions (temperature: 23°C, oxygen concentration 21%, humidity 45%, or subject to a simulated 2-h simulated flight (SF: temperature: 23°C, oxygen concentration 15%, humidity 15%, and crossed over 7 days later. Main outcome measures: clot formation and clot lysis parameters, functional platelet activation markers, and endothelial function measured by reactive hyperemia index (RHI by EndoPAT and serum microparticles.ResultsComparing baseline with SF conditions, clot maximal absorption was increased in controls (0.375 ± 0.05 vs. 0.39 ± 0.05, p < 0.05 and participants with T2DM (0.378 ± 0.089 vs. 0.397 ± 0.089, p < 0.01, while increased basal platelet activation for both fibrinogen binding and P-selectin expression (p < 0.05 was seen in participants with T2DM. Parameters of clot formation and clot lysis, stimulated platelet function (stimulated platelet response to ADP and sensitivity to prostacyclin, and endothelial function were unchanged.ConclusionWhile SF resulted in the potential of denser clot formation with enhanced basal platelet activation in T2DM, the dynamic clotting, platelet, and endothelial markers were not affected, suggesting that short-haul commercial flying adds no additional hazard for venous thromboembolism for participants with T2DM compared to controls.

  17. Experimental validation for calcul methods of structures having shock non-linearity

    International Nuclear Information System (INIS)

    Brochard, D.; Buland, P.

    1987-01-01

    For the seismic analysis of non-linear structures, numerical methods have been developed which need to be validated on experimental results. The aim of this paper is to present the design method of a test program which results will be used for this purpose. Some applications to nuclear components will illustrate this presentation [fr

  18. Examination of packaging materials in bakery products : a validated method for detection and quantification

    NARCIS (Netherlands)

    Raamsdonk, van L.W.D.; Pinckaers, V.G.Z.; Vliege, J.J.M.; Egmond, van H.J.

    2012-01-01

    Methods for the detection and quantification of packaging materials are necessary for the control of the prohibition of these materials according to Regulation (EC)767/2009. A method has been developed and validated at RIKILT for bakery products, including sweet bread and raisin bread. This choice

  19. Validation of a Novel 3-Dimensional Sonographic Method for Assessing Gastric Accommodation in Healthy Adults

    NARCIS (Netherlands)

    Buisman, Wijnand J; van Herwaarden-Lindeboom, MYA; Mauritz, Femke A; El Ouamari, Mourad; Hausken, Trygve; Olafsdottir, Edda J; van der Zee, David C; Gilja, Odd Helge

    OBJECTIVES: A novel automated 3-dimensional (3D) sonographic method has been developed for measuring gastric volumes. This study aimed to validate and assess the reliability of this novel 3D sonographic method compared to the reference standard in 3D gastric sonography: freehand magneto-based 3D

  20. Validity of a structured method of selecting abstracts for a plastic surgical scientific meeting

    NARCIS (Netherlands)

    van der Steen, LPE; Hage, JJ; Kon, M; Monstrey, SJ

    In 1999, the European Association of Plastic Surgeons accepted a structured method to assess and select the abstracts that are submitted for its yearly scientific meeting. The two criteria used to evaluate whether such a selection method is accurate were reliability and validity. The authors

  1. Application of EU guidelines for the validation of screening methods for veterinary drugs

    NARCIS (Netherlands)

    Stolker, A.A.M.

    2012-01-01

    Commission Decision (CD) 2002/657/EC describes detailed rules for method validation within the framework of residue monitoring programmes. The approach described in this CD is based on criteria. For (qualitative) screening methods, the most important criteria is that the CCß has to be below any

  2. Validity of the remote food photography method against doubly labeled water among minority preschoolers

    Science.gov (United States)

    The aim of this study was to determine the validity of energy intake (EI) estimations made using the remote food photography method (RFPM) compared to the doubly labeled water (DLW) method in minority preschool children in a free-living environment. Seven days of food intake and spot urine samples...

  3. Cross-Validation of Survival Bump Hunting by Recursive Peeling Methods.

    Science.gov (United States)

    Dazard, Jean-Eudes; Choe, Michael; LeBlanc, Michael; Rao, J Sunil

    2014-08-01

    We introduce a survival/risk bump hunting framework to build a bump hunting model with a possibly censored time-to-event type of response and to validate model estimates. First, we describe the use of adequate survival peeling criteria to build a survival/risk bump hunting model based on recursive peeling methods. Our method called "Patient Recursive Survival Peeling" is a rule-induction method that makes use of specific peeling criteria such as hazard ratio or log-rank statistics. Second, to validate our model estimates and improve survival prediction accuracy, we describe a resampling-based validation technique specifically designed for the joint task of decision rule making by recursive peeling (i.e. decision-box) and survival estimation. This alternative technique, called "combined" cross-validation is done by combining test samples over the cross-validation loops, a design allowing for bump hunting by recursive peeling in a survival setting. We provide empirical results showing the importance of cross-validation and replication.

  4. Diastolic timed Vibro-Percussion at 50 Hz delivered across a chest wall sized meat barrier enhances clot dissolution and remotely administered Streptokinase effectiveness in an in-vitro model of acute coronary thrombosis

    Directory of Open Access Journals (Sweden)

    Hoffmann Andrew

    2012-11-01

    Full Text Available Abstract Background Low Frequency Vibro-Percussion (LFVP assists clearance of thrombi in catheter systems and when applied to the heart and timed to diastole is known to enhance coronary flow. However LFVP on a clotted coronary like vessel given engagement over a chest wall sized barrier (to resemble non-invasive heart attack therapy requires study. Methods One hour old clots (n=16 were dispensed within a flexible segment of Soft-Flo catheter (4 mm lumen, weighted, interfaced with Heparinized Saline (HS, secured atop a curved dampening base, and photographed. A ~4 cm meat slab was placed over the segment and randomized to receive intermittent LFVP (engaged, - disengaged at 1 second intervals, or no LFVP for 20 minutes. HS was pulsed (~120/80 mmHg, with the diastolic phase coordinated to match LFVP delivery. The segment was then re-photographed and aspirated of fluid to determine post clot weight. The trial was then repeated with 0.5 mls of Streptokinase (15,000 IU/100 microlitre delivered ~ 2 cm upstream from the clot. Results LFVP - HS only samples (vs. controls showed; a development of clot length fluid channels absent in the control group (p Conclusion Diastolic timed LFVP (50 Hz engaged across a chest wall sized barrier enhances clot disruptive effects to an underlying coronary like system.

  5. Validation parameters of instrumental method for determination of total bacterial count in milk

    Directory of Open Access Journals (Sweden)

    Nataša Mikulec

    2004-10-01

    Full Text Available The method of flow citometry as rapid, instrumental and routine microbiological method is used for determination of total bacterial count in milk. The results of flow citometry are expressed as individual bacterial cells count. Problems regarding the interpretation of the results of total bacterial count can be avoided by transformation of the results of flow citometry method onto the scale of reference method (HRN ISO 6610:2001.. The method of flow citometry, like any analitycal method, according to the HRN EN ISO/IEC 17025:2000 standard, requires validation and verification. This paper describes parameters of validation: accuracy, precision, specificity, range, robustness and measuring uncertainty for the method of flow citometry.

  6. Interlaboratory Validation of the Leaching Environmental Assessment Framework (LEAF) Method 1313 and Method 1316

    Science.gov (United States)

    This document summarizes the results of an interlaboratory study conducted to generate precision estimates for two parallel batch leaching methods which are part of the Leaching Environmental Assessment Framework (LEAF). These methods are: (1) Method 1313: Liquid-Solid Partition...

  7. Comprehensive validation scheme for in situ fiber optics dissolution method for pharmaceutical drug product testing.

    Science.gov (United States)

    Mirza, Tahseen; Liu, Qian Julie; Vivilecchia, Richard; Joshi, Yatindra

    2009-03-01

    There has been a growing interest during the past decade in the use of fiber optics dissolution testing. Use of this novel technology is mainly confined to research and development laboratories. It has not yet emerged as a tool for end product release testing despite its ability to generate in situ results and efficiency improvement. One potential reason may be the lack of clear validation guidelines that can be applied for the assessment of suitability of fiber optics. This article describes a comprehensive validation scheme and development of a reliable, robust, reproducible and cost-effective dissolution test using fiber optics technology. The test was successfully applied for characterizing the dissolution behavior of a 40-mg immediate-release tablet dosage form that is under development at Novartis Pharmaceuticals, East Hanover, New Jersey. The method was validated for the following parameters: linearity, precision, accuracy, specificity, and robustness. In particular, robustness was evaluated in terms of probe sampling depth and probe orientation. The in situ fiber optic method was found to be comparable to the existing manual sampling dissolution method. Finally, the fiber optic dissolution test was successfully performed by different operators on different days, to further enhance the validity of the method. The results demonstrate that the fiber optics technology can be successfully validated for end product dissolution/release testing. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

  8. A simple method for validation and verification of pipettes mounted on automated liquid handlers

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Hansen, Anders Johannes; Frøslev, Tobias Guldberg

     We have implemented a simple method for validation and verification of the performance of pipettes mounted on automated liquid handlers as necessary for laboratories accredited under ISO 17025. An 8-step serial dilution of Orange G was prepared in quadruplicates in a flat bottom 96-well microtit...... available. In conclusion, we have set up a simple solution for the continuous validation of automated liquid handlers used for accredited work. The method is cheap, simple and easy to use for aqueous solutions but requires a spectrophotometer that can read microtiter plates....... We have implemented a simple method for validation and verification of the performance of pipettes mounted on automated liquid handlers as necessary for laboratories accredited under ISO 17025. An 8-step serial dilution of Orange G was prepared in quadruplicates in a flat bottom 96-well microtiter...

  9. Principles of Single-Laboratory Validation of Analytical Methods for Testing the Chemical Composition of Pesticides

    Energy Technology Data Exchange (ETDEWEB)

    Ambrus, A. [Hungarian Food Safety Office, Budapest (Hungary)

    2009-07-15

    Underlying theoretical and practical approaches towards pesticide formulation analysis are discussed, i.e. general principles, performance characteristics, applicability of validation data, verification of method performance, and adaptation of validated methods by other laboratories. The principles of single laboratory validation of analytical methods for testing the chemical composition of pesticides are outlined. Also the theoretical background is described for performing pesticide formulation analysis as outlined in ISO, CIPAC/AOAC and IUPAC guidelines, including methodological characteristics such as specificity, selectivity, linearity, accuracy, trueness, precision and bias. Appendices I–III hereof give practical and elaborated examples on how to use the Horwitz approach and formulae for estimating the target standard deviation towards acceptable analytical repeatability. The estimation of trueness and the establishment of typical within-laboratory reproducibility are treated in greater detail by means of worked-out examples. (author)

  10. 42 CFR 410.63 - Hepatitis B vaccine and blood clotting factors: Conditions.

    Science.gov (United States)

    2010-10-01

    ... 42 Public Health 2 2010-10-01 2010-10-01 false Hepatitis B vaccine and blood clotting factors... Other Health Services § 410.63 Hepatitis B vaccine and blood clotting factors: Conditions... under § 410.10, subject to the specified conditions: (a) Hepatitis B vaccine: Conditions. Effective...

  11. A constitutive model for developing blood clots with various compositions and their nonlinear viscoelastic behavior.

    Science.gov (United States)

    van Kempen, Thomas H S; Donders, Wouter P; van de Vosse, Frans N; Peters, Gerrit W M

    2016-04-01

    The mechanical properties determine to a large extent the functioning of a blood clot. These properties depend on the composition of the clot and have been related to many diseases. However, the various involved components and their complex interactions make it difficult at this stage to fully understand and predict properties as a function of the components. Therefore, in this study, a constitutive model is developed that describes the viscoelastic behavior of blood clots with various compositions. Hereto, clots are formed from whole blood, platelet-rich plasma and platelet-poor plasma to study the influence of red blood cells, platelets and fibrin, respectively. Rheological experiments are performed to probe the mechanical behavior of the clots during their formation. The nonlinear viscoelastic behavior of the mature clots is characterized using a large amplitude oscillatory shear deformation. The model is based on a generalized Maxwell model that accurately describes the results for the different rheological experiments by making the moduli and viscosities a function of time and the past and current deformation. Using the same model with different parameter values enables a description of clots with different compositions. A sensitivity analysis is applied to study the influence of parameter variations on the model output. The relative simplicity and flexibility make the model suitable for numerical simulations of blood clots and other materials showing similar behavior.

  12. A targeted ferritin-microplasmin based thrombolytic nanocage selectively dissolves blood clots.

    Science.gov (United States)

    Seo, Junyoung; Al-Hilal, Taslim A; Jee, Jun-Goo; Kim, Yong-Lim; Kim, Ha-Jeong; Lee, Byung-Heon; Kim, Soyoun; Kim, In-San

    2018-04-01

    The use of thrombolytic therapies is limited by an increased risk of systemic hemorrhage due to lysis of hemostatic clots. We sought to develop a plasmin-based thrombolytic nanocage that efficiently dissolves the clot without causing systemic fibrinolysis or disrupting hemostatic clots. Here, we generated a double chambered short-length ferritin (sFt) construct that has an N-terminal region fused to multivalent clot targeting peptides (CLT: CNAGESSKNC) and a C-terminal end fused to a microplasmin (μPn); CLT recognizes fibrin-fibronectin complexes in clots, μPn efficiently dissolves clots, and the assembly of double chambered sFt (CLT-sFt-μPn) into nanocage structure protects the activated-μPn from its circulating inhibitors. Importantly, activated CLT-sFt-μPn thrombolytic nanocage showed a prolonged circulatory life over activated-μPn and efficiently lysed the preexisting clots in both arterial and venous thromboses models. Thus, CLT-sFt-μPn thrombolytic nanocage platform represents the prototype of a targeted clot-busting agent with high efficacy and safety over existing thrombolytic therapies. Copyright © 2018 Elsevier Inc. All rights reserved.

  13. Cloning and expression of clt genes encoding milk-clotting proteases from Myxococcus xanthus 422.

    Science.gov (United States)

    Poza, M; Prieto-Alcedo, M; Sieiro, C; Villa, T G

    2004-10-01

    The screening of a gene library of the milk-clotting strain Myxococcus xanthus 422 constructed in Escherichia coli allowed the description of eight positive clones containing 26 open reading frames. Only three of them (cltA, cltB, and cltC) encoded proteins that exhibited intracellular milk-clotting ability in E. coli, Saccharomyces cerevisiae, and Pichia pastoris expression systems.

  14. A constitutive model for developing blood clots with various compositions and their nonlinear viscoelastic behavior

    NARCIS (Netherlands)

    van Kempen, T. H. S.; Donders, W. P.; van de Vosse, F. N.; Peters, G. W. M.

    2016-01-01

    The mechanical properties determine to a large extent the functioning of a blood clot. These properties depend on the composition of the clot and have been related to many diseases. However, the various involved components and their complex interactions make it difficult at this stage to fully

  15. 7 CFR 58.436 - Rennet, pepsin, other milk clotting enzymes and flavor enzymes.

    Science.gov (United States)

    2010-01-01

    ... 7 Agriculture 3 2010-01-01 2010-01-01 false Rennet, pepsin, other milk clotting enzymes and flavor enzymes. 58.436 Section 58.436 Agriculture Regulations of the Department of Agriculture (Continued... clotting enzymes and flavor enzymes. Enzyme preparations used in the manufacture of cheese shall be safe...

  16. Bayesian risk-based decision method for model validation under uncertainty

    International Nuclear Information System (INIS)

    Jiang Xiaomo; Mahadevan, Sankaran

    2007-01-01

    This paper develops a decision-making methodology for computational model validation, considering the risk of using the current model, data support for the current model, and cost of acquiring new information to improve the model. A Bayesian decision theory-based method is developed for this purpose, using a likelihood ratio as the validation metric for model assessment. An expected risk or cost function is defined as a function of the decision costs, and the likelihood and prior of each hypothesis. The risk is minimized through correctly assigning experimental data to two decision regions based on the comparison of the likelihood ratio with a decision threshold. A Bayesian validation metric is derived based on the risk minimization criterion. Two types of validation tests are considered: pass/fail tests and system response value measurement tests. The methodology is illustrated for the validation of reliability prediction models in a tension bar and an engine blade subjected to high cycle fatigue. The proposed method can effectively integrate optimal experimental design into model validation to simultaneously reduce the cost and improve the accuracy of reliability model assessment

  17. Reliability and Validity of the Footprint Assessment Method Using Photoshop CS5 Software.

    Science.gov (United States)

    Gutiérrez-Vilahú, Lourdes; Massó-Ortigosa, Núria; Costa-Tutusaus, Lluís; Guerra-Balic, Myriam

    2015-05-01

    Several sophisticated methods of footprint analysis currently exist. However, it is sometimes useful to apply standard measurement methods of recognized evidence with an easy and quick application. We sought to assess the reliability and validity of a new method of footprint assessment in a healthy population using Photoshop CS5 software (Adobe Systems Inc, San Jose, California). Forty-two footprints, corresponding to 21 healthy individuals (11 men with a mean ± SD age of 20.45 ± 2.16 years and 10 women with a mean ± SD age of 20.00 ± 1.70 years) were analyzed. Footprints were recorded in static bipedal standing position using optical podography and digital photography. Three trials for each participant were performed. The Hernández-Corvo, Chippaux-Smirak, and Staheli indices and the Clarke angle were calculated by manual method and by computerized method using Photoshop CS5 software. Test-retest was used to determine reliability. Validity was obtained by intraclass correlation coefficient (ICC). The reliability test for all of the indices showed high values (ICC, 0.98-0.99). Moreover, the validity test clearly showed no difference between techniques (ICC, 0.99-1). The reliability and validity of a method to measure, assess, and record the podometric indices using Photoshop CS5 software has been demonstrated. This provides a quick and accurate tool useful for the digital recording of morphostatic foot study parameters and their control.

  18. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations

    OpenAIRE

    Jihan M Badr

    2013-01-01

    Background: Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. Materials and Method: In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Ha...

  19. Intrinsic clotting factors in dependency of age, sex, body mass index, and oral contraceptives: definition and risk of elevated clotting factor levels.

    Science.gov (United States)

    Luxembourg, Beate; Schmitt, Joern; Humpich, Marek; Glowatzki, Matthias; Seifried, Erhard; Lindhoff-Last, Edelgard

    2009-10-01

    Elevated clotting factors have been demonstrated to be a risk factor for venous thromboembolism (VTE). The aim of our study was to investigate the impact of age, sex, body mass index, and oral contraceptives on the clotting factor activities of factors VIII, IX, XI, and XII and their impact on the cutoff definition and risk of VTE associated with elevated clotting factors. Factor VIII, IX, XI, and XII activities were measured in 499 blood donors and 286 patients with VTE. Age and body mass index predicted significantly and independently the clotting factor activities of factors VIII, IX, and XI, whereas use of oral contraceptives predicted factor IX, XI, and XII levels. Percentiles of clotting factor activities, which are often used for the cutoff definition of elevated clotting factors, varied due to the effect of age, body mass index, and oral contraceptives. The adjusted odds ratios for VTE were 10.3 [95% confidence interval (CI) 5.1-20.7], 6.1 (95% CI 3.1-12.0), and 3.3 (95% CI 1.9-5.8) for elevated factors VIII, IX, and XI, respectively. Furthermore, our study demonstrates for the first time that elevated factor XII is associated with an increased risk of VTE (adjusted odds ratio 2.9, 95% CI 1.6-5.3).

  20. Performance Validity Testing in Neuropsychology: Methods for Measurement Development and Maximizing Diagnostic Accuracy.

    Science.gov (United States)

    Wodushek, Thomas R; Greher, Michael R

    2017-05-01

    In the first column in this 2-part series, Performance Validity Testing in Neuropsychology: Scientific Basis and Clinical Application-A Brief Review, the authors introduced performance validity tests (PVTs) and their function, provided a justification for why they are necessary, traced their ongoing endorsement by neuropsychological organizations, and described how they are used and interpreted by ever increasing numbers of clinical neuropsychologists. To enhance readers' understanding of these measures, this second column briefly describes common detection strategies used in PVTs as well as the typical methods used to validate new PVTs and determine cut scores for valid/invalid determinations. We provide a discussion of the latest research demonstrating how neuropsychologists can combine multiple PVTs in a single battery to improve sensitivity/specificity to invalid responding. Finally, we discuss future directions for the research and application of PVTs.

  1. Validation of Experimental whole-body SAR Assessment Method in a Complex Indoor Environment

    DEFF Research Database (Denmark)

    Bamba, Aliou; Joseph, Wout; Vermeeren, Gunter

    2012-01-01

    Assessing experimentally the whole-body specific absorption rate (SARwb) in a complex indoor environment is very challenging. An experimental method based on room electromagnetics theory (accounting only the Line-Of-Sight as specular path) to assess the whole-body SAR is validated by numerical...... of the proposed method is that it allows discarding the computation burden because it does not use any discretizations. Results show good agreement between measurement and computation at 2.8 GHz, as long as the plane wave assumption is valid, i.e., for high distances from the transmitter. Relative deviations 0...

  2. A chromatographic method validation to quantify tablets Mephenesine of national production

    International Nuclear Information System (INIS)

    Suarez Perez, Yania; Izquierdo Castro, Adalberto; Milian Sanchez, Jana Daria

    2009-01-01

    Authors made validation of an analytical method by high performance liquid chromatography (HPLC) for quantification of Mephenesine in recently reformulated 500 mg tablets. With regard to its application to quality control, validation included the following parameters: linearity, accuracy, precision, and selectivity. Results were satisfactory within 50-150 % rank. In the case of its use in subsequent studies of chemical stability, the selectivity for stability and sensitivity was assessed. Estimated detection and quantification limits were appropriate, and the method was selective versus the possible degradation products. (Author)

  3. 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 methods apply equally well to particles of different suppliers. In trueness testing, information whether the particle size distribution has changed during analysis is required. Results are largely expected to follow normal distributions due to the expected high number of particles. An approach...... approach for the validation of methods for detection and quantification of nanoparticles in food samples. It proposes validation of identity, selectivity, precision, working range, limit of detection and robustness, bearing in mind that each “result” must include information about the chemical identity...

  4. Reduced clot debris size using standing waves formed via high intensity focused ultrasound

    Science.gov (United States)

    Guo, Shifang; Du, Xuan; Wang, Xin; Lu, Shukuan; Shi, Aiwei; Xu, Shanshan; Bouakaz, Ayache; Wan, Mingxi

    2017-09-01

    The feasibility of utilizing high intensity focused ultrasound (HIFU) to induce thrombolysis has been demonstrated previously. However, clinical concerns still remain related to the clot debris produced via fragmentation of the original clot potentially being too large and hence occluding downstream vessels, causing hazardous emboli. This study investigates the use of standing wave fields formed via HIFU to disintegrate the thrombus while achieving a reduced clot debris size in vitro. The results showed that the average diameter of the clot debris calculated by volume percentage was smaller in the standing wave mode than in the travelling wave mode at identical ultrasound thrombolysis settings. Furthermore, the inertial cavitation dose was shown to be lower in the standing wave mode, while the estimated cavitation bubble size distribution was similar in both modes. These results show that a reduction of the clot debris size with standing waves may be attributed to the particle trapping of the acoustic potential well which contributed to particle fragmentation.

  5. In vivo chicken model for peripheral intravascular human fibrin clot detection

    International Nuclear Information System (INIS)

    Hui, K.Y.

    1988-01-01

    A chicken model was prepared that provides a simple and economical method of evaluating the use of fibrin-specific monoclonal antibody 64C5 in the detection of peripheral vascular thrombi. Human fibrin was clotted in segments of a chicken's femoral artery and vein prior to intravenous injection of radioiodinated antibody 64C5. After a 3-hr perfusion time, the thrombosed and contralateral control segments of the vessels were excised and counted for radioactivity. The radiolabeled 64C5 uptake ratio of the thrombosed segment to the control segment was 5.4 +/- 1.2 (p less than 0.007) in the femoral artery, and 3.8 +/- 1.1 (p less than 0.02) in the femoral vein. This in vivo chicken model may also find application in studies of targeting agents for human fibrin

  6. 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)

  7. A Comparison of Three Methods for the Analysis of Skin Flap Viability: Reliability and Validity.

    Science.gov (United States)

    Tim, Carla Roberta; Martignago, Cintia Cristina Santi; da Silva, Viviane Ribeiro; Dos Santos, Estefany Camila Bonfim; Vieira, Fabiana Nascimento; Parizotto, Nivaldo Antonio; Liebano, Richard Eloin

    2018-05-01

    Objective: Technological advances have provided new alternatives to the analysis of skin flap viability in animal models; however, the interrater validity and reliability of these techniques have yet to be analyzed. The present study aimed to evaluate the interrater validity and reliability of three different methods: weight of paper template (WPT), paper template area (PTA), and photographic analysis. Approach: Sixteen male Wistar rats had their cranially based dorsal skin flap elevated. On the seventh postoperative day, the viable tissue area and the necrotic area of the skin flap were recorded using the paper template method and photo image. The evaluation of the percentage of viable tissue was performed using three methods, simultaneously and independently by two raters. The analysis of interrater reliability and viability was performed using the intraclass correlation coefficient and Bland Altman Plot Analysis was used to visualize the presence or absence of systematic bias in the evaluations of data validity. Results: The results showed that interrater reliability for WPT, measurement of PTA, and photographic analysis were 0.995, 0.990, and 0.982, respectively. For data validity, a correlation >0.90 was observed for all comparisons made between the three methods. In addition, Bland Altman Plot Analysis showed agreement between the comparisons of the methods and the presence of systematic bias was not observed. Innovation: Digital methods are an excellent choice for assessing skin flap viability; moreover, they make data use and storage easier. Conclusion: Independently from the method used, the interrater reliability and validity proved to be excellent for the analysis of skin flaps' viability.

  8. Development and validation of stability indicating UPLC assay method for ziprasidone active pharma ingredient

    Directory of Open Access Journals (Sweden)

    Sonam Mittal

    2012-01-01

    Full Text Available Background: Ziprasidone, a novel antipsychotic, exhibits a potent highly selective antagonistic activity on D2 and 5HT2A receptors. Literature survey for ziprasidone revealed several analytical methods based on different techniques but no UPLC method has been reported so far. Aim: Aim of this research paper is to present a simple and rapid stability indicating isocratic, ultra performance liquid chromatographic (UPLC method which was developed and validated for the determination of ziprasidone active pharmaceutical ingredient. Forced degradation studies of ziprasidone were studied under acid, base, oxidative hydrolysis, thermal stress and photo stress conditions. Materials and Methods: The quantitative determination of ziprasidone drug was performed on a Supelco analytical column (100×2.1 mm i.d., 2.7 ΅m with 10 mM ammonium acetate buffer (pH: 6.7 and acetonitrile (ACN as mobile phase with the ratio (55:45-Buffer:ACN at a flow rate of 0.35 ml/ min. For UPLC method, UV detection was made at 318 nm and the run time was 3 min. Developed UPLC method was validated as per ICH guidelines. Results and Conclusion: Mild degradation of the drug substance was observed during oxidative hydrolysis and considerable degradation observed during basic hydrolysis. During method validation, parameters such as precision, linearity, ruggedness, stability, robustness, and specificity were evaluated, which remained within acceptable limits. Developed UPLC method was successfully applied for evaluating assay of Ziprasidone active Pharma ingredient.

  9. Validated UV-Spectrophotometric Methods for Determination of Gemifloxacin Mesylate in Pharmaceutical Tablet Dosage Forms

    Directory of Open Access Journals (Sweden)

    R. Rote Ambadas

    2010-01-01

    Full Text Available Two simple, economic and accurate UV spectrophotometric methods have been developed for determination of gemifloxacin mesylate in pharmaceutical tablet formulation. The first UV-spectrophotometric method depends upon the measurement of absorption at the wavelength 263.8 nm. In second area under curve method the wavelength range for detection was selected from 268.5-258.5 nm. Beer’s law was obeyed in the range of 2 to 12 μgmL-1 for both the methods. The proposed methods was validated statistically and applied successfully to determination of gemifloxacin mesylate in pharmaceutical formulation.

  10. Method of administration of PROMIS scales did not significantly impact score level, reliability, or validity

    DEFF Research Database (Denmark)

    Bjorner, Jakob B; Rose, Matthias; Gandek, Barbara

    2014-01-01

    OBJECTIVES: To test the impact of the method of administration (MOA) on score level, reliability, and validity of scales developed in the Patient Reported Outcomes Measurement Information System (PROMIS). STUDY DESIGN AND SETTING: Two nonoverlapping parallel forms each containing eight items from......, no significant mode differences were found and all confidence intervals were within the prespecified minimal important difference of 0.2 standard deviation. Parallel-forms reliabilities were very high (ICC = 0.85-0.93). Only one across-mode ICC was significantly lower than the same-mode ICC. Tests of validity...... questionnaire (PQ), personal digital assistant (PDA), or personal computer (PC) and a second form by PC, in the same administration. Method equivalence was evaluated through analyses of difference scores, intraclass correlations (ICCs), and convergent/discriminant validity. RESULTS: In difference score analyses...

  11. Method validation for uranium content analysis using a potentiometer T-90

    International Nuclear Information System (INIS)

    Torowati; Ngatijo; Rahmiati

    2016-01-01

    An experimental method validation has been conducted for uranium content analysis using Potentiometer T-90. The method validation experiment was performed in the quality control laboratory of Experiment Fuel Element Installation, PTBBN - BATAN. The objective is to determine the level of precision and accuracy of analytical results for uranium analysis referring to the latest American Standard Test Method (ASTM) of ASTM C1267-11, which is a modified reference method by reducing of reagent consumption by 10% of the amount used by the original method. The ASTM C 1267-11 reference is a new ASTM as a substitute for the older ASTM namely ASTM C799, Vol.12.01, 2003. It is, therefore, necessary to validate the renewed method. The tool used for the analysis of uranium was potentiometer T-90 and the material used was standard uranium oxide powder CRM (Certificate Reference Material). Validation of the method was done by analyzing standard uranium powder by 7 times weighing and 7 times analysis. Analysis results were used to determine the level of accuracy, precision, Relative Standard Deviation (RSD) and Horwitz coefficient Variation and limit detection and quantitation. The average uranium obtained for this method validation is 84.36% with Standard Deviation (SD) of 0.12%, Relative Standard Deviation (RSD) 0.14% and 2/3 Horwitz coefficient Variation (CV Horwitz) 2.05%. The results show that RSD value is smaller than the value of (2/3) CV Horwitz, which means that this method has a high precision. The accuracy value obtained is 0.48%, and since the acceptance limit of high level of accuracy is when the accuracy value is <2.00%, this method is regarded as having a high degree of accuracy [1]. The limit of detection (LOD) and and the limit of quantitation (LOQ) are 0.0145 g/L and 0.0446 g/L respectively. It is concluded that the ASTM C 1267-11 reference method is valid for use. (author)

  12. Clotting of mammalian fibrinogens by papain: a re-examination.

    Science.gov (United States)

    Doolittle, Russell F

    2014-10-28

    Papain has long been known to cause the gelation of mammalian fibrinogens. It has also been reported that papain-fibrin is insoluble in dispersing solvents like strong urea or sodium bromide solutions, similar to what is observed with thrombin-generated clots in the presence of factor XIIIa and calcium. In those old studies, both the gelation and subsequent clot stabilization were attributed to papain, although the possibility that the second step might be due to contaminating factor XIII in fibrinogen preparations was considered. I have revisited this problem in light of knowledge acquired over the past half-century about thiol proteases like papain, which mostly cleave peptide bonds, and transglutaminases like factor XIIIa that catalyze the formation of ε-lysyl-γ-glutamyl cross-links. Recombinant fibrinogen, inherently free of factor XIII and other plasma proteins, formed a stable gel when treated with papain alone. Sodium dodecyl sulfate-polyacrylamide gel electrophoresis revealed that the intermolecular cross-linking in papain-fibrin leads to γ-chain dimers, trimers, and tetramers, just as is the case with thrombin-factor XIIIa-stabilized fibrin. Mass spectrometry of bands excised from gels showed that the cross-linked material is quite different from what occurs with factor XIIIa, however. With papain, the cross-linking occurs between γ chains in neighboring protofibrils becoming covalently linked in a "head-to-tail" fashion by a transpeptidation reaction involving the α-amino group of γ-Tyr1 and a papain cleavage site at γ-Gly403 near the carboxy terminus, rather than by the (reciprocal) "tail-to-tail" manner that occurs with factor XIIIa and that depends on cross-links between γ-Lys406 and γ-Gln398.

  13. Methods and procedures for the verification and validation of artificial neural networks

    CERN Document Server

    Taylor, Brian J

    2006-01-01

    Neural networks are members of a class of software that have the potential to enable intelligent computational systems capable of simulating characteristics of biological thinking and learning. This volume introduces some of the methods and techniques used for the verification and validation of neural networks and adaptive systems.

  14. Review of seismic tests for qualification of components and validation of methods

    International Nuclear Information System (INIS)

    Buland, P.; Gantenbein, F.; Gibert, R.J.; Hoffmann, A.; Queval, J.C.

    1988-01-01

    Seismic tests are performed in CEA-DEMT since many years in order: to demonstrate the qualification of components, to give an experimental validation of calculation methods used for seismic design of components. The paper presents examples of these two types of tests, a description of the existing facilities and details about the new facility TAMARIS under construction. (author)

  15. A validation framework for microbial forensic methods based on statistical pattern recognition

    Energy Technology Data Exchange (ETDEWEB)

    Velsko, S P

    2007-11-12

    This report discusses a general approach to validating microbial forensic methods that attempt to simultaneously distinguish among many hypotheses concerning the manufacture of a questioned biological agent sample. It focuses on the concrete example of determining growth medium from chemical or molecular properties of a bacterial agent to illustrate the concepts involved.

  16. Validation of the DLW method in Japanese quail at different water fluxes using laser and IRMS

    NARCIS (Netherlands)

    van Trigt, R; Kerstel, E.R.T.; Neubert, R.E.M.; Meijer, H.A.J.; Mclean, M.; Visser, G.H.

    2002-01-01

    In Japanese quail (Coturnix c. japonica; n = 9), the doubly labeled water (DLW) method (H-2, O-18) for estimation Of CO2 production (1/day) was validated. To evaluate its sensitivity to water efflux levels (r(H2Oe); g/day) and to assumptions of fractional evaporative water loss (x; dimensionless),

  17. Likelihood ratio data to report the validation of a forensic fingerprint evaluation method

    NARCIS (Netherlands)

    Ramos, Daniel; Haraksim, Rudolf; Meuwly, Didier

    2017-01-01

    Data to which the authors refer to throughout this article are likelihood ratios (LR) computed from the comparison of 5–12 minutiae fingermarks with fingerprints. These LRs data are used for the validation of a likelihood ratio (LR) method in forensic evidence evaluation. These data present a

  18. Validation of the ultraviolet spectrophotometry method for the quality control of ciprofloxacin chlorhydrate in Ciprecu tablets

    International Nuclear Information System (INIS)

    Perez Navarro, Maikel; Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania

    2014-01-01

    Quinolones are a group of antimicrobials of high clinical significance. Ciprofloxacin hydrochloride monohydrate is a second-generation antibacterial fluoroquinolone for treatment of several infections and is marketed as eye drops, injections, capsule and tablets. To develop and to validate an ultraviolet spectrophotometric analytical method to be used in the quality control of ciprofloxacin hydrochloride monohydrate in newly manufactured Ciprecu tablets

  19. Measurement and data analysis methods for field-scale wind erosion studies and model validation

    NARCIS (Netherlands)

    Zobeck, T.M.; Sterk, G.; Funk, R.F.; Rajot, J.L.; Stout, J.E.; Scott Van Pelt, R.

    2003-01-01

    Accurate and reliable methods of measuring windblown sediment are needed to confirm, validate, and improve erosion models, assess the intensity of aeolian processes and related damage, determine the source of pollutants, and for other applications. This paper outlines important principles to

  20. Validity of a Simulation Game as a Method for History Teaching

    Science.gov (United States)

    Corbeil, Pierre; Laveault, Dany

    2011-01-01

    The aim of this research is, first, to determine the validity of a simulation game as a method of teaching and an instrument for the development of reasoning and, second, to study the relationship between learning and students' behavior toward games. The participants were college students in a History of International Relations course, with two…

  1. A guideline for the validation of likelihood ratio methods used for forensic evidence evaluation

    NARCIS (Netherlands)

    Meuwly, Didier; Ramos, Daniel; Haraksim, Rudolf

    2017-01-01

    This Guideline proposes a protocol for the validation of forensic evaluation methods at the source level, using the Likelihood Ratio framework as defined within the Bayes’ inference model. In the context of the inference of identity of source, the Likelihood Ratio is used to evaluate the strength of

  2. Validation of the actuator line method using near wake measurements of the MEXICO rotor

    DEFF Research Database (Denmark)

    Nilsson, Karl; Shen, Wen Zhong; Sørensen, Jens Nørkær

    2015-01-01

    The purpose of the present work is to validate the capability of the actuator line method to compute vortex structures in the near wake behind the MEXICO experimental wind turbine rotor. In the MEXICO project/MexNext Annex, particle image velocimetry measurements have made it possible to determine...

  3. Validity Argument for Assessing L2 Pragmatics in Interaction Using Mixed Methods

    Science.gov (United States)

    Youn, Soo Jung

    2015-01-01

    This study investigates the validity of assessing L2 pragmatics in interaction using mixed methods, focusing on the evaluation inference. Open role-plays that are meaningful and relevant to the stakeholders in an English for Academic Purposes context were developed for classroom assessment. For meaningful score interpretations and accurate…

  4. Review of seismic tests for qualification of components and validation of methods

    Energy Technology Data Exchange (ETDEWEB)

    Buland, P; Gantenbein, F; Gibert, R J; Hoffmann, A; Queval, J C [CEA-CEN SACLAY-DEMT, Gif sur Yvette-Cedex (France)

    1988-07-01

    Seismic tests are performed in CEA-DEMT since many years in order: to demonstrate the qualification of components, to give an experimental validation of calculation methods used for seismic design of components. The paper presents examples of these two types of tests, a description of the existing facilities and details about the new facility TAMARIS under construction. (author)

  5. Validity and reliability of a method for assessment of cervical vertebral maturation.

    Science.gov (United States)

    Zhao, Xiao-Guang; Lin, Jiuxiang; Jiang, Jiu-Hui; Wang, Qingzhu; Ng, Sut Hong

    2012-03-01

    To evaluate the validity and reliability of the cervical vertebral maturation (CVM) method with a longitudinal sample. Eighty-six cephalograms from 18 subjects (5 males and 13 females) were selected from the longitudinal database. Total mandibular length was measured on each film; an increased rate served as the gold standard in examination of the validity of the CVM method. Eleven orthodontists, after receiving intensive training in the CVM method, evaluated all films twice. Kendall's W and the weighted kappa statistic were employed. Kendall's W values were higher than 0.8 at both times, indicating strong interobserver reproducibility, but interobserver agreement was documented twice at less than 50%. A wide range of intraobserver agreement was noted (40.7%-79.1%), and substantial intraobserver reproducibility was proved by kappa values (0.53-0.86). With regard to validity, moderate agreement was reported between the gold standard and observer staging at the initial time (kappa values 0.44-0.61). However, agreement seemed to be unacceptable for clinical use, especially in cervical stage 3 (26.8%). Even though the validity and reliability of the CVM method proved statistically acceptable, we suggest that many other growth indicators should be taken into consideration in evaluating adolescent skeletal maturation.

  6. Alternative method to validate the seasonal land cover regions of the conterminous United States

    Science.gov (United States)

    Zhiliang Zhu; Donald O. Ohlen; Raymond L. Czaplewski; Robert E. Burgan

    1996-01-01

    An accuracy assessment method involving double sampling and the multivariate composite estimator has been used to validate the prototype seasonal land cover characteristics database of the conterminous United States. The database consists of 159 land cover classes, classified using time series of 1990 1-km satellite data and augmented with ancillary data including...

  7. A systematic review of validated methods to capture acute bronchospasm using administrative or claims data.

    Science.gov (United States)

    Sharifi, Mona; Krishanswami, Shanthi; McPheeters, Melissa L

    2013-12-30

    To identify and assess billing, procedural, or diagnosis code, or pharmacy claim-based algorithms used to identify acute bronchospasm in administrative and claims databases. We searched the MEDLINE database from 1991 to September 2012 using controlled vocabulary and key terms related to bronchospasm, wheeze and acute asthma. We also searched the reference lists of included studies. Two investigators independently assessed the full text of studies against pre-determined inclusion criteria. Two reviewers independently extracted data regarding participant and algorithm characteristics. Our searches identified 677 citations of which 38 met our inclusion criteria. In these 38 studies, the most commonly used ICD-9 code was 493.x. Only 3 studies reported any validation methods for the identification of bronchospasm, wheeze or acute asthma in administrative and claims databases; all were among pediatric populations and only 2 offered any validation statistics. Some of the outcome definitions utilized were heterogeneous and included other disease based diagnoses, such as bronchiolitis and pneumonia, which are typically of an infectious etiology. One study offered the validation of algorithms utilizing Emergency Department triage chief complaint codes to diagnose acute asthma exacerbations with ICD-9 786.07 (wheezing) revealing the highest sensitivity (56%), specificity (97%), PPV (93.5%) and NPV (76%). There is a paucity of studies reporting rigorous methods to validate algorithms for the identification of bronchospasm in administrative data. The scant validated data available are limited in their generalizability to broad-based populations. Copyright © 2013 Elsevier Ltd. All rights reserved.

  8. Update of Standard Practices for New Method Validation in Forensic Toxicology.

    Science.gov (United States)

    Wille, Sarah M R; Coucke, Wim; De Baere, Thierry; Peters, Frank T

    2017-01-01

    International agreement concerning validation guidelines is important to obtain quality forensic bioanalytical research and routine applications as it all starts with the reporting of reliable analytical data. Standards for fundamental validation parameters are provided in guidelines as those from the US Food and Drug Administration (FDA), the European Medicines Agency (EMA), the German speaking Gesellschaft fur Toxikologie und Forensische Chemie (GTFCH) and the Scientific Working Group of Forensic Toxicology (SWGTOX). These validation parameters include selectivity, matrix effects, method limits, calibration, accuracy and stability, as well as other parameters such as carryover, dilution integrity and incurred sample reanalysis. It is, however, not easy for laboratories to implement these guidelines into practice as these international guidelines remain nonbinding protocols, that depend on the applied analytical technique, and that need to be updated according the analyst's method requirements and the application type. In this manuscript, a review of the current guidelines and literature concerning bioanalytical validation parameters in a forensic context is given and discussed. In addition, suggestions for the experimental set-up, the pros and cons of statistical approaches and adequate acceptance criteria for the validation of bioanalytical applications are given. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  9. MR-based water content estimation in cartilage: design and validation of a method

    DEFF Research Database (Denmark)

    Shiguetomi Medina, Juan Manuel; Kristiansen, Maja Sophie; Ringgaard, Steffen

    Purpose: Design and validation of an MR-based method that allows the calculation of the water content in cartilage tissue. Methods and Materials: Cartilage tissue T1 map based water content MR sequences were used on a 37 Celsius degree stable system. The T1 map intensity signal was analyzed on 6...... cartilage samples from living animals (pig) and on 8 gelatin samples which water content was already known. For the data analysis a T1 intensity signal map software analyzer used. Finally, the method was validated after measuring and comparing 3 more cartilage samples in a living animal (pig). The obtained...... map based water content sequences can provide information that, after being analyzed using a T1-map analysis software, can be interpreted as the water contained inside a cartilage tissue. The amount of water estimated using this method was similar to the one obtained at the dry-freeze procedure...

  10. GC Method Validation for the Analysis of Menthol in Suppository Pharmaceutical Dosage Form

    Directory of Open Access Journals (Sweden)

    Murad N. Abualhasan

    2017-01-01

    Full Text Available Menthol is widely used as a fragrance and flavor in the food and cosmetic industries. It is also used in the medical and pharmaceutical fields for its various biological effects. Gas chromatography (GC is considered to be a sensitive method for the analysis of menthol. GC chromatographic separation was developed using capillary column (VF-624 and a flame ionization detector (FID. The method was validated as per ICH guidelines for various parameters such as precision, linearity, accuracy, solution stability, robustness, limit of detection, and quantification. The tested validation parameters were found to be within acceptable limits. The method was successfully applied for the quantification of menthol in suppositories formulations. Quality control departments and official pharmacopeias can use our developed method in the analysis of menthol in pharmaceutical dosage formulation and raw material.

  11. Low-cost extrapolation method for maximal LTE radio base station exposure estimation: test and validation.

    Science.gov (United States)

    Verloock, Leen; Joseph, Wout; Gati, Azeddine; Varsier, Nadège; Flach, Björn; Wiart, Joe; Martens, Luc

    2013-06-01

    An experimental validation of a low-cost method for extrapolation and estimation of the maximal electromagnetic-field exposure from long-term evolution (LTE) radio base station installations are presented. No knowledge on downlink band occupation or service characteristics is required for the low-cost method. The method is applicable in situ. It only requires a basic spectrum analyser with appropriate field probes without the need of expensive dedicated LTE decoders. The method is validated both in laboratory and in situ, for a single-input single-output antenna LTE system and a 2×2 multiple-input multiple-output system, with low deviations in comparison with signals measured using dedicated LTE decoders.

  12. Low-cost extrapolation method for maximal lte radio base station exposure estimation: Test and validation

    International Nuclear Information System (INIS)

    Verloock, L.; Joseph, W.; Gati, A.; Varsier, N.; Flach, B.; Wiart, J.; Martens, L.

    2013-01-01

    An experimental validation of a low-cost method for extrapolation and estimation of the maximal electromagnetic-field exposure from long-term evolution (LTE) radio base station installations are presented. No knowledge on down-link band occupation or service characteristics is required for the low-cost method. The method is applicable in situ. It only requires a basic spectrum analyser with appropriate field probes without the need of expensive dedicated LTE decoders. The method is validated both in laboratory and in situ, for a single-input single-output antenna LTE system and a 2x2 multiple-input multiple-output system, with low deviations in comparison with signals measured using dedicated LTE decoders. (authors)

  13. Validation of three new methods for determination of metal emissions using a modified Environmental Protection Agency Method 301

    Energy Technology Data Exchange (ETDEWEB)

    Catherine A. Yanca; Douglas C. Barth; Krag A. Petterson; Michael P. Nakanishi; John A. Cooper; Bruce E. Johnsen; Richard H. Lambert; Daniel G. Bivins [Cooper Environmental Services, LLC, Portland, OR (United States)

    2006-12-15

    Three new methods applicable to the determination of hazardous metal concentrations in stationary source emissions were developed and evaluated for use in U.S. Environmental Protection Agency (EPA) compliance applications. Two of the three independent methods, a continuous emissions monitor-based method (Xact) and an X-ray-based filter method (XFM), are used to measure metal emissions. The third method involves a quantitative aerosol generator (QAG), which produces a reference aerosol used to evaluate the measurement methods. A modification of EPA Method 301 was used to validate the three methods for As, Cd, Cr, Pb, and Hg, representing three hazardous waste combustor Maximum Achievable Control Technology (MACT) metal categories (low volatile, semivolatile, and volatile). The measurement methods were evaluated at a hazardous waste combustor (HWC) by comparing measured with reference aerosol concentrations. The QAG, Xact, and XFM met the modified Method 301 validation criteria. All three of the methods demonstrated precisions and accuracies on the order of 5%. The measurement methods should be applicable to emissions from a wide range of sources, and the reference aerosol generator should be applicable to additional analytes. EPA recently approved an alternative monitoring petition for an HWC at Eli Lilly's Tippecanoe site in Lafayette, IN, in which the Xact is used for demonstrating compliance with the HWC MACT metal emissions (low volatile, semivolatile, and volatile). The QAG reference aerosol generator was approved as a method for providing a quantitative reference aerosol, which is required for certification and continuing quality assurance of the Xact. 30 refs., 5 figs., 11 tabs.

  14. Validation of the quality control methods for active ingredients of Fungirex cream

    International Nuclear Information System (INIS)

    Perez Navarro, Maikel; Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania

    2014-01-01

    Fungirex cream is a two-drug product, that is, undecylenic acid and zinc undecylenate over a suitable basis. Since this is a product not documented in the official monographs of the pharmacopoeia, simple analytical methods were suggested for quantitation of analytes of interest in the cream, which are useful for release of newly prepared cream batches. To validate two volumetric methods for the quality control of active ingredients in Fungirex cream

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

    OpenAIRE

    Sunil Kumar Yelamanchi V; Useni Reddy Mallu; I. V Kasi Viswanath; D. Balasubramanyam; G. Narshima Murthy

    2016-01-01

    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...

  16. Validation of the quality control method for sodium dicloxacillin in Dicloxen capsules

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Perez Navarro, Maikel; Suarez Perez, Yania

    2014-01-01

    Sodium dicloxacillin is a semi synthetic derivative of the isoxasocyl penicillin group that may appear in oral suspension form and in caplets. For the analysis of the raw materials and the finished products, it is recommended to use high performance liquid chromatography that is an unavailable method at the dicloxen capsule manufacturing lab for the routine analysis of the drug. To develop and to validate a useful ultraviolet spectrophotometry method for the quality control of sodium dicloxacillin in Dicloxen capsules

  17. Interlaboratory Validation of the Leaching Environmental Assessment Framework (LEAF) Method 1314 and Method 1315

    Science.gov (United States)

    This report summarizes the results of an interlaboratory study conducted to generate precision estimates for two leaching methods under review by the U.S. EPA’s OSWER for inclusion into the EPA’s SW-846: Method 1314: Liquid-Solid Partitioning as a Function of Liquid...

  18. Validation of methods for the determination of radium in waters and soil

    International Nuclear Information System (INIS)

    Decaillon, J.-G.; Bickel, M.; Hill, C.; Altzitzoglou, T.

    2004-01-01

    This article describes the advantages and disadvantages of several analytical methods used to prepare the alpha-particle source. As a result of this study, a new method combining commercial extraction and ion chromatography prior to a final co-precipitation step is proposed. This method has been applied and validated on several matrices (soil, waters) in the framework of international intercomparisons. The integration of this method in a global procedure to analyze actinoids and radium from a single solution (or digested soil) is also described

  19. Validation of uncertainty of weighing in the preparation of radionuclide standards by Monte Carlo Method

    International Nuclear Information System (INIS)

    Cacais, F.L.; Delgado, J.U.; Loayza, V.M.

    2016-01-01

    In preparing solutions for the production of radionuclide metrology standards is necessary measuring the quantity Activity by mass. The gravimetric method by elimination is applied to perform weighing with smaller uncertainties. At this work is carried out the validation, by the Monte Carlo method, of the uncertainty calculation approach implemented by Lourenco and Bobin according to ISO GUM for the method by elimination. The results obtained by both uncertainty calculation methods were consistent indicating that were fulfilled the conditions for the application of ISO GUM in the preparation of radioactive standards. (author)

  20. Validation of ascorbic acid tablets of national production by igh-performance liquid chromatography method

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Izquierdo Castro, Idalberto

    2009-01-01

    We validate an analytical method by high-performance liquid chromatography to determine ascorbic acid proportion in vitamin C tablets, which was designed as an alternative method to quality control and to follow-up of active principle chemical stability, since official techniques to quality control of ascorbic acid in tablets are not selective with degradation products. Method was modified according to that reported in USP 28, 2005 for analysis of injectable product. We used a RP-18 column of 250 x 4.6 mm 5 μm with a UV detector to 245 nm. Its validation was necessary for both objectives, considering parameters required for methods of I and II categories. This method was enough linear, exact, and precise in the rank of 100-300 μg/mL. Also, it was selective with remaining components of matrix and with the possible degradation products achieved in stressing conditions. Detection and quantification limits were estimated. When method was validated it was applied to ascorbic acid quantification in two batches of expired tablets and we detected a marked influence of container in active degradation principle after 12 months at room temperature. (Author)

  1. High-performance liquid chromatography method validation for determination of tetracycline residues in poultry meat

    Directory of Open Access Journals (Sweden)

    Vikas Gupta

    2014-01-01

    Full Text Available Background: In this study, a method for determination of tetracycline (TC residues in poultry with the help of high-performance liquid chromatography technique was validated. Materials and Methods: The principle step involved in ultrasonic-assisted extraction of TCs from poultry samples by 2 ml of 20% trichloroacetic acid and phosphate buffer (pH 4, which gave a clearer supernatant and high recovery, followed by centrifugation and purification by using 0.22 μm filter paper. Results: Validity study of the method revealed that all obtained calibration curves showed good linearity (r2 > 0.999 over the range of 40-4500 ng. Sensitivity was found to be 1.54 and 1.80 ng for oxytetracycline (OTC and TC. Accuracy was in the range of 87.94-96.20% and 72.40-79.84% for meat. Precision was lower than 10% in all cases indicating that the method can be used as a validated method. Limit of detection was found to be 4.8 and 5.10 ng for OTC and TC, respectively. The corresponding values of limit of quantitation were 11 and 12 ng. Conclusion: The method reliably identifies and quantifies the selected TC and OTC in the reconstituted poultry meat in the low and sub-nanogram range and can be applied in any laboratory.

  2. Method validation for simultaneous counting of Total α , β in Drinking Water using Liquid Scintillation Counter

    International Nuclear Information System (INIS)

    Al-Masri, M. S.; Nashawati, A.

    2014-05-01

    In this work, Method Validation Methods and Pulse Shape Analysis were validated to determine gross Alpha and Beta Emitters in Drinking Water using Liquid Scintillation Counter Win spectral 1414. Validation parameters include Method Detection Limit, Method Quantitation Limit, Repeatability Limit, Intermediate Precision, Trueness) Bias), Recovery Coefficient, Linearity and Uncertainty Budget in analysis. The results show that the Method Detection Limit and Method Quantitation Limit were 0.07, 0.24 Bq/l for Alpha emitters respectively, and 0.42, 1.4 Bq/l for Beta emitters, respectively. The relative standard deviation of Repeatability Limit reached 2.81% for Alpha emitters and 3.96% for Beta emitters. In addition to, the relative standard deviation of Intermediate Precisionis was 0.54% for Alpha emitters and 1.17% for Beta emitters. Moreover, the trueness was - 7.7% for Alpha emitters and - 4.5% for Beta emitters. Recovery Coefficient ranged between 87 - 96% and 88-101 for Alpha and Beta emitters, respectively. Linearity reached 1 for both Alpha and Beta emitters. on the other hand, Uncertainty Budget for all continents was 96.65% ,83.14% for Alpha and Beta emitters, respectively (author).

  3. Iodinated Contrast Does Not Alter Clotting Dynamics in Acute Ischemic Stroke as Measured by Thromboelastography

    Science.gov (United States)

    McDonald, Mark M; Archeval-Lao, Joancy M; Cai, Chunyan; Peng, Hui; Sangha, Navdeep; Parker, Stephanie A; Wetzel, Jeremy; Riney, Stephen A; Cherches, Matt F; Guthrie, Greer J; Roper, Tiffany C; Kawano-Castillo, Jorge F; Pandurengan, Renga; Rahbar, Mohammad H; Grotta, James C

    2014-01-01

    Background and Purpose Iodinated contrast agents used for computed tomography angiography (CTA) may alter fibrin fiber characteristics and decrease fibrinolysis by tissue plasminogen activator (tPA). Thromboelastography (TEG™) measures the dynamics of coagulation and correlates with thrombolysis in acute ischemic stroke (AIS) patients. We hypothesized that receiving CTA prior to tPA will not impair thrombolysis as measured by TEG™. Methods AIS patients receiving 0.9 mg/kg tPA within 4.5 hours of symptom onset were prospectively enrolled. For CTA, 350 mg/dL of iohexol or 320 mg/dL of iodixanol at a dose of 2.2 ml/kg was administered. TEG™ was measured prior to tPA and 10-minutes after tPA bolus. CTA timing was left to the discretion of the treating physician. Results Of 136 AIS patients who received tPA, 47 had CTA prior to tPA bolus, and 42 had either CTA following tPA and post-tPA TEG™ draw or no CTA (non-contrast group). The median change in clot lysis (LY30) following tPA was 95.3% in the contrast group vs. 95.0% in the non-contrast group (p = 0.74). Thus, tPA-induced thrombolysis did not differ between contrast and non-contrast groups. Additionally, there was no effect of contrast on any pre-tPA TEG™ value. Conclusions Our data do not support an effect of iodinated contrast agents on clot formation or tPA activity. PMID:24370757

  4. Three phase partitioning of zingibain, a milk-clotting enzyme from Zingiber officinale Roscoe rhizomes.

    Science.gov (United States)

    Gagaoua, Mohammed; Hoggas, Naouel; Hafid, Kahina

    2015-02-01

    The present work describes for the first time an elegant non-chromatographic method, the three phase partitioning for the purification and recovery of zingibain, a milk-clotting enzyme, from Zingiber officinale rhizomes. Factors affecting partitioning efficiency such as (NH4)2SO4 saturation, crude extract to t-butanol ratio and pH on zingibain partitioning were investigated. Optimal purification parameters were 50% (NH4)2SO4 saturation with 1.0:1.0 ratio of crude extract:t-butanol at pH 7.0, which gave 14.91 purification fold with 215% recovery of zingibain. The enzyme was found to be exclusively partitioned in the aqueous phase. The enzyme showed a prominent single band on SDS-PAGE. It is a monomeric protein of 33.8 kDa and its isoelectric point is 4.38. The enzyme exhibited maximal proteolytic activity at a temperature of 60 °C and pH 7.0. It was found to be stable at 40-65 °C during 2 h. The enzyme was found to be highly stable against numerous metal ions and its activity was enhanced by Ca(2+), K(+) and Na(+). It was completely inhibited by heavy metal ions such as Cu(2+) and Hg(2+) and partially by Cd(+). Zingibain milk-clotting activity (MCA) was found to be highly stable when stored under freezing (-20 °C) for 30 days compared at 4 °C. Copyright © 2014 Elsevier B.V. All rights reserved.

  5. 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...... extraction methods. However. PLE was the preferred extraction method because the method can be highly automated, use only small amounts of solvents, provide the cleanest extracts, and allow the extraction of light and oxygen-sensitive flavonoids to be carried out in an inert atmosphere protected from light......-step PLE method showed good selectivity, precision (RSDs = 3.1-11%) and recovery of the extractable flavonoids (98-99%). The method also appeared to be a multi-method, i.e. generally applicable to, e.g. phenolic acids in potatoes and carrots....

  6. Developing and validating a nutrition knowledge questionnaire: key methods and considerations.

    Science.gov (United States)

    Trakman, Gina Louise; Forsyth, Adrienne; Hoye, Russell; Belski, Regina

    2017-10-01

    To outline key statistical considerations and detailed methodologies for the development and evaluation of a valid and reliable nutrition knowledge questionnaire. Literature on questionnaire development in a range of fields was reviewed and a set of evidence-based guidelines specific to the creation of a nutrition knowledge questionnaire have been developed. The recommendations describe key qualitative methods and statistical considerations, and include relevant examples from previous papers and existing nutrition knowledge questionnaires. Where details have been omitted for the sake of brevity, the reader has been directed to suitable references. We recommend an eight-step methodology for nutrition knowledge questionnaire development as follows: (i) definition of the construct and development of a test plan; (ii) generation of the item pool; (iii) choice of the scoring system and response format; (iv) assessment of content validity; (v) assessment of face validity; (vi) purification of the scale using item analysis, including item characteristics, difficulty and discrimination; (vii) evaluation of the scale including its factor structure and internal reliability, or Rasch analysis, including assessment of dimensionality and internal reliability; and (viii) gathering of data to re-examine the questionnaire's properties, assess temporal stability and confirm construct validity. Several of these methods have previously been overlooked. The measurement of nutrition knowledge is an important consideration for individuals working in the nutrition field. Improved methods in the development of nutrition knowledge questionnaires, such as the use of factor analysis or Rasch analysis, will enable more confidence in reported measures of nutrition knowledge.

  7. Assessment of Advanced Life Support competence when combining different test methods--reliability and validity

    DEFF Research Database (Denmark)

    Ringsted, C; Lippert, F; Hesselfeldt, R

    2007-01-01

    Cardiac Arrest Simulation Test (CASTest) scenarios for the assessments according to guidelines 2005. AIMS: To analyse the reliability and validity of the individual sub-tests provided by ERC and to find a combination of MCQ and CASTest that provides a reliable and valid single effect measure of ALS...... that possessed high reliability, equality of test sets, and ability to discriminate between the two groups of supposedly different ALS competence. CONCLUSIONS: ERC sub-tests of ALS competence possess sufficient reliability and validity. A combined ALS score with equal weighting of one MCQ and one CASTest can...... competence. METHODS: Two groups of participants were included in this randomised, controlled experimental study: a group of newly graduated doctors, who had not taken the ALS course (N=17) and a group of students, who had passed the ALS course 9 months before the study (N=16). Reliability in terms of inter...

  8. A simple method for validation and verification of pipettes mounted on automated liquid handlers

    DEFF Research Database (Denmark)

    Stangegaard, Michael; Hansen, Anders Johannes; Frøslev, Tobias G

    2011-01-01

    We have implemented a simple, inexpensive, and fast procedure for validation and verification of the performance of pipettes mounted on automated liquid handlers (ALHs) as necessary for laboratories accredited under ISO 17025. A six- or seven-step serial dilution of OrangeG was prepared in quadru......We have implemented a simple, inexpensive, and fast procedure for validation and verification of the performance of pipettes mounted on automated liquid handlers (ALHs) as necessary for laboratories accredited under ISO 17025. A six- or seven-step serial dilution of OrangeG was prepared...... are freely available. In conclusion, we have set up a simple, inexpensive, and fast solution for the continuous validation of ALHs used for accredited work according to the ISO 17025 standard. The method is easy to use for aqueous solutions but requires a spectrophotometer that can read microtiter plates....

  9. MR-based Water Content Estimation in Cartilage: Design and Validation of a Method

    DEFF Research Database (Denmark)

    Shiguetomi Medina, Juan Manuel; Kristiansen, Maja Sofie; Ringgaard, Steffen

    2012-01-01

    Objective Design and validation of an MR-based method that allows the calculation of the water content in cartilage tissue. Material and Methods We modified and adapted to cartilage tissue T1 map based water content MR sequences commonly used in the neurology field. Using a 37 Celsius degree stable...... was costumed and programmed. Finally, we validated the method after measuring and comparing 3 more cartilage samples in a living animal (pig). The obtained data was analyzed and the water content calculated. Then, the same samples were freeze-dried (this technique allows to take out all the water that a tissue...... contains) and we measured the water they contained. Results We could reproduce twice the 37 Celsius degree system and could perform the measurements in a similar way. We found that the MR T1 map based water content sequences can provide information that, after being analyzed with a special software, can...

  10. A Validated RP-HPLC Method for the Determination of Atazanavir in Pharmaceutical Dosage Form

    Directory of Open Access Journals (Sweden)

    K. Srinivasu

    2011-01-01

    Full Text Available A validated RP HPLC method for the estimation of atazanavir in capsule dosage form on YMC ODS 150 × 4.6 mm, 5 μ column using mobile phase composition of ammonium dihydrogen phosphate buffer (pH 2.5 with acetonitrile (55:45 v/v. Flow rate was maintained at 1.5 mL/min with 288 nm UV detection. The retention time obtained for atazanavir was at 4.7 min. The detector response was linear in the concentration range of 30 - 600 μg/mL. This method has been validated and shown to be specific, sensitive, precise, linear, accurate, rugged, robust and fast. Hence, this method can be applied for routine quality control of atazanavir in capsule dosage forms as well as in bulk drug.

  11. A Validated, Rapid HPLC-ESI-MS/MS Method for the Determination of Lycopsamine.

    Science.gov (United States)

    Jedlinszki, Nikoletta; Csupor, Dezső

    2015-07-01

    The aim of the present work was to develop and validate an HPLC-MS/MS method for the determination of a major pyrrolizidine alkaloid of comfrey (lycopsamine) in aqueous samples as a basis for the development of a method for the determination of absorption of lycopsamine by human skin. A linear calibration curve was established in the range of 1.32-440 ng. The intraday precision during the 3-day validation period ranged between 0.57 and 2.48% while the interday precision was 1.70% and 1.95% for quality control samples. LOD was 0.014 ng and recovery was above 97%. The lycopsamine content of the samples stored for 9 and 25 days at 22 degrees C, 10 degrees C and -25 degrees C did not vary. These results underline the good repeatability and accuracy of our method and allow the analysis of samples with very low lycopsamine content.

  12. Uncertainty estimates of purity measurements based on current information: toward a "live validation" of purity methods.

    Science.gov (United States)

    Apostol, Izydor; Kelner, Drew; Jiang, Xinzhao Grace; Huang, Gang; Wypych, Jette; Zhang, Xin; Gastwirt, Jessica; Chen, Kenneth; Fodor, Szilan; Hapuarachchi, Suminda; Meriage, Dave; Ye, Frank; Poppe, Leszek; Szpankowski, Wojciech

    2012-12-01

    To predict precision and other performance characteristics of chromatographic purity methods, which represent the most widely used form of analysis in the biopharmaceutical industry. We have conducted a comprehensive survey of purity methods, and show that all performance characteristics fall within narrow measurement ranges. This observation was used to develop a model called Uncertainty Based on Current Information (UBCI), which expresses these performance characteristics as a function of the signal and noise levels, hardware specifications, and software settings. We applied the UCBI model to assess the uncertainty of purity measurements, and compared the results to those from conventional qualification. We demonstrated that the UBCI model is suitable to dynamically assess method performance characteristics, based on information extracted from individual chromatograms. The model provides an opportunity for streamlining qualification and validation studies by implementing a "live validation" of test results utilizing UBCI as a concurrent assessment of measurement uncertainty. Therefore, UBCI can potentially mitigate the challenges associated with laborious conventional method validation and facilitates the introduction of more advanced analytical technologies during the method lifecycle.

  13. Determination of vitamin C in foods: current state of method validation.

    Science.gov (United States)

    Spínola, Vítor; Llorent-Martínez, Eulogio J; Castilho, Paula C

    2014-11-21

    Vitamin C is one of the most important vitamins, so reliable information about its content in foodstuffs is a concern to both consumers and quality control agencies. However, the heterogeneity of food matrixes and the potential degradation of this vitamin during its analysis create enormous challenges. This review addresses the development and validation of high-performance liquid chromatography methods for vitamin C analysis in food commodities, during the period 2000-2014. The main characteristics of vitamin C are mentioned, along with the strategies adopted by most authors during sample preparation (freezing and acidification) to avoid vitamin oxidation. After that, the advantages and handicaps of different analytical methods are discussed. Finally, the main aspects concerning method validation for vitamin C analysis are critically discussed. Parameters such as selectivity, linearity, limit of quantification, and accuracy were studied by most authors. Recovery experiments during accuracy evaluation were in general satisfactory, with usual values between 81 and 109%. However, few methods considered vitamin C stability during the analytical process, and the study of the precision was not always clear or complete. Potential future improvements regarding proper method validation are indicated to conclude this review. Copyright © 2014. Published by Elsevier B.V.

  14. Validation of analytical methods for the stability studies of naproxen suppositories for infant and adult use

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Garcia Pulpeiro, Oscar

    2011-01-01

    Analytical and validating studies were performed in this paper, with a view to using them in the stability studies of the future formulations of naproxen suppositories for children and adults. The most influential factors in the naproxen stability were determined, that is, the major degradation occurred in acid medium, oxidative medium and by light action. One high-performance liquid chromatography-based method was evaluated, which proved to be adequate to quantify naproxen in suppositories and was selective against degradation products. The quantification limit was 3,480 μg, so it was valid for these studies. Additionally, the parameters specificity for stability, detection and quantification limits were evaluated for the direct semi-aqueous acid-base method, which was formerly validated for the quality control and showed satisfactory results. Nevertheless, the volumetric methods were not regarded as stability indicators; therefore, this method will be used along with the chromatographic methods of choice, that is, thin-layer chromatography and highperformance liquid chromatography, to determine the degradation products

  15. Validation method for determination of cholesterol in human urine with electrochemical sensors using gold electrodes

    Science.gov (United States)

    Riyanto, Laksono, Tomy Agung

    2017-12-01

    Electrochemical sensors for the determination of cholesterol with Au as a working electrode (Au) and its application to the analysis of urine have been done. The gold electrode was prepared using gold pure (99.99%), with size 1.0 mm by length and wide respectively, connected with silver wire using silver conductive paint. Validation methods have been investigated in the analysis of cholesterol in human urine using electrochemical sensors or cyclic voltammetry (CV) method. The effect of electrolyte and uric acid concentration has been determined to produce the optimum method. Validation method parameters for cholesterol analysis in human urine using CV are precision, recovery, linearity, limit of detection (LOD) and limit of quantification (LOQ). The result showed the correlation of concentration of cholesterol to anodic peak current is the coefficient determination of R2 = 0.916. The results of the validation method showed the precision, recovery, linearity, LOD, and LOQ are 1.2539%, 144.33%, 0.916, 1.49 × 10-1 mM and 4.96 × 10-1 mM, respectively. As a conclusion is Au electrode is a good electrode for electrochemical sensors to determination of cholesterol in human urine.

  16. Contribution to the validation of thermal ratchetting prevision methods in metallic structures; Contribution a la validation des methodes de prevision du rochet thermique dans les structures metalliques

    Energy Technology Data Exchange (ETDEWEB)

    Rakotovelo, A.M

    1998-03-01

    This work concerns the steady state assessment in the metallic structures subjected to thermomechanical cyclic loadings in biaxial stress state. The effect of the short time mechanical overloads is also investigated. The first chapter is devoted to a bibliographic research concerning the behaviour of the materials and the structures in the cyclic plasticity. Some works relate to the experimental aspect as well as the numerical one for the steady state assessment of such structures are presented. The experimental part of the study is presented in the second chapter. The experimental device was carried out in order to prescribe tension and torsion forces combined with cyclic thermal loading. Some tests was then carried out, among these tests certain include some overloads in tension or torsion. The last chapter describes the numerical calculations using different models (linear isotropic hardening, linear kinematic hardening and elasto-viscoplastic Chaboche's model) and the application of some simplified methods for the ratchetting assessment in the structures. We have considered two categories of methods. The first one is based on an elastic analysis (Bree's diagram, 3 Sm rule, efficiency rule) and the second one combines elastic analysis and elastoplastic analysis of the first cycle (Gatt's and Taleb's methods). The results of this study have enabled: to validate in the biaxial stress state an expression which takes into account the effect of mechanical short time overloads; to test the performances of considered models to describe the evolution of the structure during the first cycle and to take into account the effect of short time overloads. Among the considered models, the elastoplastic Chaboche's model seems to be the most accurate to describe the structure's behaviour during the first cycles; to validate some simplified methods. Certain methods based only on elastic analysis (Bee's diagram and efficiency rule) seem not

  17. 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. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Estimating Rooftop Suitability for PV: A Review of Methods, Patents, and Validation Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Melius, J. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Margolis, R. [National Renewable Energy Lab. (NREL), Golden, CO (United States); Ong, S. [National Renewable Energy Lab. (NREL), Golden, CO (United States)

    2013-12-01

    A number of methods have been developed using remote sensing data to estimate rooftop area suitable for the installation of photovoltaics (PV) at various geospatial resolutions. This report reviews the literature and patents on methods for estimating rooftop-area appropriate for PV, including constant-value methods, manual selection methods, and GIS-based methods. This report also presents NREL's proposed method for estimating suitable rooftop area for PV using Light Detection and Ranging (LiDAR) data in conjunction with a GIS model to predict areas with appropriate slope, orientation, and sunlight. NREL's method is validated against solar installation data from New Jersey, Colorado, and California to compare modeled results to actual on-the-ground measurements.

  19. Development and validation of a multiresidue method for pesticide analysis in honey by UFLC-MS

    Directory of Open Access Journals (Sweden)

    Adriana M. Zamudio S.

    2017-05-01

    Full Text Available A method for the determination of pesticide residues in honey by ultra fast liquid chromatography coupled with mass spectrometry was developed. For this purpose, different variations of the QuECHERS method were performed: (i amount of sample, (ii type of salt to control pH, (iii buffer pH, and (iv different mixtures for cleaning-up. In addition, to demonstrate that the method is reliable, different validation parameters were studied: accuracy, limits of detection and quantification, linearity and selectivity. The results showed that by means of the changes introduced it was possible to get a more selective method that improves the accuracy of about 19 pesticides selected from the original method. It was found that the method is suitable for the analysis of 50 pesticides, out of 56. Furthermore, with the developed method recoveries between 70 and 120% and relative standard deviation below 15% were found.

  20. Development and Statistical Validation of Spectrophotometric Methods for the Estimation of Nabumetone in Tablet Dosage Form

    Directory of Open Access Journals (Sweden)

    A. R. Rote

    2010-01-01

    Full Text Available Three new simple, economic spectrophotometric methods were developed and validated for the estimation of nabumetone in bulk and tablet dosage form. First method includes determination of nabumetone at absorption maxima 330 nm, second method applied was area under curve for analysis of nabumetone in the wavelength range of 326-334 nm and third method was First order derivative spectra with scaling factor 4. Beer law obeyed in the concentration range of 10-30 μg/mL for all three methods. The correlation coefficients were found to be 0.9997, 0.9998 and 0.9998 by absorption maxima, area under curve and first order derivative spectra. Results of analysis were validated statistically and by performing recovery studies. The mean percent recoveries were found satisfactory for all three methods. The developed methods were also compared statistically using one way ANOVA. The proposed methods have been successfully applied for the estimation of nabumetone in bulk and pharmaceutical tablet dosage form.

  1. Review on Laryngeal Palpation Methods in Muscle Tension Dysphonia: Validity and Reliability Issues.

    Science.gov (United States)

    Khoddami, Seyyedeh Maryam; Ansari, Noureddin Nakhostin; Jalaie, Shohreh

    2015-07-01

    Laryngeal palpation is a common clinical method for the assessment of neck and laryngeal muscles in muscle tension dysphonia (MTD). To review the available laryngeal palpation methods used in patients with MTD for the assessment, diagnosis, or document of treatment outcomes. A systematic review of the literature concerning palpatory methods in MTD was conducted using the databases MEDLINE (PubMed), ScienceDirect, Scopus, Web of science, Web of knowledge and Cochrane Library between July and October 2013. Relevant studies were identified by one reviewer based on screened titles/abstracts and full texts. Manual searching was also used to track the source literature. There were five main as well as miscellaneous palpation methods that were different according to target anatomical structures, judgment or grading system, and using tasks. There were only a few scales available, and the majority of the palpatory methods were qualitative. Most of the palpatory methods evaluate the tension at both static and dynamic tasks. There was little information about the validity and reliability of the available methods. The literature on the scientific evidence of muscle tension indicators perceived by laryngeal palpation in MTD is scarce. Future studies should be conducted to investigate the validity and reliability of palpation methods. Copyright © 2015 The Voice Foundation. Published by Elsevier Inc. All rights reserved.

  2. Validity Evaluation of the Assessment Method for Postural Loading on the Upper Body in Printing Industry

    Directory of Open Access Journals (Sweden)

    Mohammad Khandan

    2016-07-01

    Full Text Available Background and Objectives: Musculoskeletal disorders and injuries are known as a global occupational challenge. These injuries are more are concentrated in the upper limb. There are several methods to assess this kind of disorders, each of which have different efficiencies for various jobs based on their strengths and weaknesses. This study aimed to assess the validity of LUBA method in order to evaluate risk factors for musculoskeletal disorders in a printing industry in Qom province, 2014. Methods: In this descriptive cross-sectional study, all operational workers (n=94 were investigated in 2014. Nordic Musculoskeletal Questionnaire (NMQ was used to collect data on musculoskeletal disorders. We also used LUBA method to analyze postures in four different parts of the body (neck, shoulder, elbow, and wrist. The obtained data were analyzed using Mann-Whitney, Kruskal Wallis, and Kappa agreement tests. Results: Lumbar region of back with 35.1% prevalence had the most problems. The results of LUBA method showed that most postures were located at the second corrective action level, and need further studies. Agreement between assessment of shoulder posture and its disorders was significant (p0.05.  Conclusion: According to the results of this study on reliability and predictive validity of the LUBA method in printing industry, it can be concluded that this method is not a reliable method for posture assessment; however, further and more comprehensive studies are recommended.  

  3. Development of a benchtop baking method for chemically leavened crackers. II. Validation of the method

    Science.gov (United States)

    A benchtop baking method has been developed to predict the contribution of gluten functionality to overall flour performance for chemically leavened crackers. Using a diagnostic formula and procedure, dough rheology was analyzed to evaluate the extent of gluten development during mixing and machinin...

  4. Validity of the Remote Food Photography Method against Doubly Labeled Water among Minority Preschoolers

    OpenAIRE

    Nicklas, Theresa; Saab, Rabab; Islam, Noemi G.; Wong, William; Butte, Nancy; Schulin, Rebecca; Liu, Yan; Apolzan, John W.; Myers, Candice A.; Martin, Corby K.

    2017-01-01

    Objective To determine the validity of energy intake (EI) estimations made using the Remote Food Photography Method (RFPM) compared to the doubly-labeled water (DLW) method in minority preschool children in a free-living environment. Methods Seven days of food intake and spot urine samples excluding first void collections for DLW analysis were obtained on 39 3-to-5 year old Hispanic and African American children. Using an iPhone, caregivers captured before and after pictures of the child’s in...

  5. A statistical method (cross-validation) for bone loss region detection after spaceflight

    Science.gov (United States)

    Zhao, Qian; Li, Wenjun; Li, Caixia; Chu, Philip W.; Kornak, John; Lang, Thomas F.

    2010-01-01

    Astronauts experience bone loss after the long spaceflight missions. Identifying specific regions that undergo the greatest losses (e.g. the proximal femur) could reveal information about the processes of bone loss in disuse and disease. Methods for detecting such regions, however, remains an open problem. This paper focuses on statistical methods to detect such regions. We perform statistical parametric mapping to get t-maps of changes in images, and propose a new cross-validation method to select an optimum suprathreshold for forming clusters of pixels. Once these candidate clusters are formed, we use permutation testing of longitudinal labels to derive significant changes. PMID:20632144

  6. A method of knowledge base verification and validation for nuclear power plants expert systems

    International Nuclear Information System (INIS)

    Kwon, Il Won

    1996-02-01

    The adoption of expert systems mainly as operator supporting systems is becoming increasingly popular as the control algorithms of system become more and more sophisticated and complicated. As a result of this popularity, a large number of expert systems are developed. The nature of expert systems, however, requires that they be verified and validated carefully and that detailed methodologies for their development be devised. Therefore, it is widely noted that assuring the reliability of expert systems is very important, especially in nuclear industry, and it is also recognized that the process of verification and validation is an essential part of reliability assurance for these systems. Research and practices have produced numerous methods for expert system verification and validation (V and V) that suggest traditional software and system approaches to V and V. However, many approaches and methods for expert system V and V are partial, unreliable, and not uniform. The purpose of this paper is to present a new approach to expert system V and V, based on Petri nets, providing a uniform model. We devise and suggest an automated tool, called COKEP (Checker Of Knowledge base using Extended Petri net), for checking incorrectness, inconsistency, and incompleteness in a knowledge base. We also suggest heuristic analysis for validation process to show that the reasoning path is correct

  7. Modelling of the activity system - development of an evaluation method for integrated system validation

    International Nuclear Information System (INIS)

    Norros, Leena; Savioja, Paula

    2004-01-01

    In this paper we present our recent research which focuses on creating an evaluation method for human-system interfaces of complex systems. The method is aimed for use in the validation of modernised nuclear power plant (NPP) control rooms, and other complex systems with high reliability requirements. The task in validation is to determine whether the human-system functions safely and effectively. This question can be operationalized to the selection of relevant operational features and their appropriate acceptance criteria. Thus, there is a need to ensure that the results of the evaluation can be generalized so that they serve the purpose of integrated system validation. The definition of the appropriate acceptance criteria provides basis for the judgement of the appropriateness of the performance of the system. We propose that the operational situations and the acceptance criteria should be defined based on modelling of the NPP operation that is comprehended as an activity system. We developed a new core-tasks modelling framework. It is a formative modelling approach that combines causal, functional and understanding explanations of system performance. In this paper we reason how modelling can be used as a medium to determine the validity of the emerging control room system. (Author)

  8. Development and Validation of High Performance Liquid Chromatography Method for Determination Atorvastatin in Tablet

    Science.gov (United States)

    Yugatama, A.; Rohmani, S.; Dewangga, A.

    2018-03-01

    Atorvastatin is the primary choice for dyslipidemia treatment. Due to patent expiration of atorvastatin, the pharmaceutical industry makes copy of the drug. Therefore, the development methods for tablet quality tests involving atorvastatin concentration on tablets needs to be performed. The purpose of this research was to develop and validate the simple atorvastatin tablet analytical method by HPLC. HPLC system used in this experiment consisted of column Cosmosil C18 (150 x 4,6 mm, 5 µm) as the stationary reverse phase chomatography, a mixture of methanol-water at pH 3 (80:20 v/v) as the mobile phase, flow rate of 1 mL/min, and UV detector at wavelength of 245 nm. Validation methods were including: selectivity, linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). The results of this study indicate that the developed method had good validation including selectivity, linearity, accuracy, precision, LOD, and LOQ for analysis of atorvastatin tablet content. LOD and LOQ were 0.2 and 0.7 ng/mL, and the linearity range were 20 - 120 ng/mL.

  9. Method for Pre-Conditioning a Measured Surface Height Map for Model Validation

    Science.gov (United States)

    Sidick, Erkin

    2012-01-01

    This software allows one to up-sample or down-sample a measured surface map for model validation, not only without introducing any re-sampling errors, but also eliminating the existing measurement noise and measurement errors. Because the re-sampling of a surface map is accomplished based on the analytical expressions of Zernike-polynomials and a power spectral density model, such re-sampling does not introduce any aliasing and interpolation errors as is done by the conventional interpolation and FFT-based (fast-Fourier-transform-based) spatial-filtering method. Also, this new method automatically eliminates the measurement noise and other measurement errors such as artificial discontinuity. The developmental cycle of an optical system, such as a space telescope, includes, but is not limited to, the following two steps: (1) deriving requirements or specs on the optical quality of individual optics before they are fabricated through optical modeling and simulations, and (2) validating the optical model using the measured surface height maps after all optics are fabricated. There are a number of computational issues related to model validation, one of which is the "pre-conditioning" or pre-processing of the measured surface maps before using them in a model validation software tool. This software addresses the following issues: (1) up- or down-sampling a measured surface map to match it with the gridded data format of a model validation tool, and (2) eliminating the surface measurement noise or measurement errors such that the resulted surface height map is continuous or smoothly-varying. So far, the preferred method used for re-sampling a surface map is two-dimensional interpolation. The main problem of this method is that the same pixel can take different values when the method of interpolation is changed among the different methods such as the "nearest," "linear," "cubic," and "spline" fitting in Matlab. The conventional, FFT-based spatial filtering method used to

  10. A Sensitive Validated Spectrophotometric Method for the Determination of Flucloxacillin Sodium

    Directory of Open Access Journals (Sweden)

    R. Singh Gujral

    2009-01-01

    Full Text Available A simple and sensitive spectrophotometric method has been proposed for the determination of flucloxacillin sodium. The determination method is based on charge transfer complexation reaction of the drug with iodine in methanol-dichloromethane medium. The absorbance was measured at 362 nm against the reagent blank. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges 1-9 μg/mL for flucloxacillin. The method was validated for specificity, linearity, precision, accuracy. The degree of linearity of the calibration curves, the percent recoveries, limit of detection and quantitation for the spectrophotometric method were determined. No interferences could be observed from the additives commonly present in the pharmaceutical formulations. The method was successfully applied for in vitro determination of human urine samples with low RSD value. This is simple, specific, accurate and sensitive spectrophotometric method.

  11. Validation of a method to measure plutonium levels in marine sediments in Cuba

    International Nuclear Information System (INIS)

    Sibello Hernández, Rita Y.; Cartas Aguila, Héctor A.; Cozzella, María Letizia

    2008-01-01

    The main objective of this research was to develop and to validate a method of radiochemical separation of plutonium, suitable from the economic and practical point of view, in Cuba conditions. This method allowed to determine plutonium activity levels in the marine sediments from Cienfuegos Bay. The selected method of radiochemical separation was that of anionic chromatography and the measure technique was the quadrupole inductively coupled plasma mass spectrometry. The method was applied to a certified reference material, six repetitions were carried out and a good correspondence between the average measured value and the average certified value of plutonium was achieved, so the trueness of the method was demonstrated. It was also proven the precision of the method, since it was obtained a variation coefficient of 11% at 95% confidence level. The obtained results show that the presence of plutonium in the analyzed marine sediment samples is only due to the global radioactive fallout. (author)

  12. Experimental validation of the buildings energy performance (PEC assessment methods with reference to occupied spaces heating

    Directory of Open Access Journals (Sweden)

    Cristian PETCU

    2010-01-01

    Full Text Available This paper is part of the series of pre-standardization research aimed to analyze the existing methods of calculating the Buildings Energy Performance (PEC in view of their correction of completing. The entire research activity aims to experimentally validate the PEC Calculation Algorithm as well as the comparative application, on the support of several case studies focused on representative buildings of the stock of buildings in Romania, of the PEC calculation methodology for buildings equipped with occupied spaces heating systems. The targets of the report are the experimental testing of the calculation models so far known (NP 048-2000, Mc 001-2006, SR EN 13790:2009, on the support provided by the CE INCERC Bucharest experimental building, together with the complex calculation algorithms specific to the dynamic modeling, for the evaluation of the occupied spaces heat demand in the cold season, specific to the traditional buildings and to modern buildings equipped with solar radiation passive systems, of the ventilated solar space type. The schedule of the measurements performed in the 2008-2009 cold season is presented as well as the primary processing of the measured data and the experimental validation of the heat demand monthly calculation methods, on the support of CE INCERC Bucharest. The calculation error per heating season (153 days of measurements between the measured heat demand and the calculated one was of 0.61%, an exceptional value confirming the phenomenological nature of the INCERC method, NP 048-2006. The mathematical model specific to the hourly thermal balance is recurrent – decisional with alternating paces. The experimental validation of the theoretical model is based on the measurements performed on the CE INCERC Bucharest building, within a time lag of 57 days (06.01-04.03.2009. The measurements performed on the CE INCERC Bucharest building confirm the accuracy of the hourly calculation model by comparison to the values

  13. In Vitro Dissolution Profile of Dapagliflozin: Development, Method Validation, and Analysis of Commercial Tablets

    Directory of Open Access Journals (Sweden)

    Rafaela Zielinski Cavalheiro de Meira

    2017-01-01

    Full Text Available Dapagliflozin was the first of its class (inhibitors of sodium-glucose cotransporter to be approved in Europe, USA, and Brazil. As the drug was recently approved, there is the need for research on analytical methods, including dissolution studies for the quality evaluation and assurance of tablets. The dissolution methodology was developed with apparatus II (paddle in 900 mL of medium (simulated gastric fluid, pH 1.2, temperature set at 37±0.5°C, and stirring speed of 50 rpm. For the quantification, a spectrophotometric (λ=224 nm method was developed and validated. In validation studies, the method proved to be specific and linear in the range from 0.5 to 15 μg·mL−1 (r2=0.998. The precision showed results with RSD values lower than 2%. The recovery of 80.72, 98.47, and 119.41% proved the accuracy of the method. Through a systematic approach by applying Factorial 23, the robustness of the method was confirmed (p>0.05. The studies of commercial tablets containing 5 or 10 mg demonstrated that they could be considered similar through f1, f2, and dissolution efficiency analyses. Also, the developed method can be used for the quality evaluation of dapagliflozin tablets and can be considered as a scientific basis for future official pharmacopoeial methods.

  14. Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form

    Science.gov (United States)

    Khattab, Fatma I.; Ramadan, Nesrin K.; Hegazy, Maha A.; Al-Ghobashy, Medhat A.; Ghoniem, Nermine S.

    2015-03-01

    Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D1) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD1) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D1 at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL-1 and 0.5-10.0 μg mL-1 for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method.

  15. Establishing survey validity and reliability for American Indians through "think aloud" and test-retest methods.

    Science.gov (United States)

    Hauge, Cindy Horst; Jacobs-Knight, Jacque; Jensen, Jamie L; Burgess, Katherine M; Puumala, Susan E; Wilton, Georgiana; Hanson, Jessica D

    2015-06-01

    The purpose of this study was to use a mixed-methods approach to determine the validity and reliability of measurements used within an alcohol-exposed pregnancy prevention program for American Indian women. To develop validity, content experts provided input into the survey measures, and a "think aloud" methodology was conducted with 23 American Indian women. After revising the measurements based on this input, a test-retest was conducted with 79 American Indian women who were randomized to complete either the original measurements or the new, modified measurements. The test-retest revealed that some of the questions performed better for the modified version, whereas others appeared to be more reliable for the original version. The mixed-methods approach was a useful methodology for gathering feedback on survey measurements from American Indian participants and in indicating specific survey questions that needed to be modified for this population. © The Author(s) 2015.

  16. Reference Proteome Extracts for Mass Spec Instrument Performance Validation and Method Development

    Science.gov (United States)

    Rosenblatt, Mike; Urh, Marjeta; Saveliev, Sergei

    2014-01-01

    Biological samples of high complexity are required to test protein mass spec sample preparation procedures and validate mass spec instrument performance. Total cell protein extracts provide the needed sample complexity. However, to be compatible with mass spec applications, such extracts should meet a number of design requirements: compatibility with LC/MS (free of detergents, etc.)high protein integrity (minimal level of protein degradation and non-biological PTMs)compatibility with common sample preparation methods such as proteolysis, PTM enrichment and mass-tag labelingLot-to-lot reproducibility Here we describe total protein extracts from yeast and human cells that meet the above criteria. Two extract formats have been developed: Intact protein extracts with primary use for sample preparation method development and optimizationPre-digested extracts (peptides) with primary use for instrument validation and performance monitoring

  17. Software phantom with realistic speckle modeling for validation of image analysis methods in echocardiography

    Science.gov (United States)

    Law, Yuen C.; Tenbrinck, Daniel; Jiang, Xiaoyi; Kuhlen, Torsten

    2014-03-01

    Computer-assisted processing and interpretation of medical ultrasound images is one of the most challenging tasks within image analysis. Physical phenomena in ultrasonographic images, e.g., the characteristic speckle noise and shadowing effects, make the majority of standard methods from image analysis non optimal. Furthermore, validation of adapted computer vision methods proves to be difficult due to missing ground truth information. There is no widely accepted software phantom in the community and existing software phantoms are not exible enough to support the use of specific speckle models for different tissue types, e.g., muscle and fat tissue. In this work we propose an anatomical software phantom with a realistic speckle pattern simulation to _ll this gap and provide a exible tool for validation purposes in medical ultrasound image analysis. We discuss the generation of speckle patterns and perform statistical analysis of the simulated textures to obtain quantitative measures of the realism and accuracy regarding the resulting textures.

  18. Validation of cleaning method for various parts fabricated at a Beryllium facility

    Energy Technology Data Exchange (ETDEWEB)

    Davis, Cynthia M. [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2015-12-15

    This study evaluated and documented a cleaning process that is used to clean parts that are fabricated at a beryllium facility at Los Alamos National Laboratory. The purpose of evaluating this cleaning process was to validate and approve it for future use to assure beryllium surface levels are below the Department of Energy’s release limits without the need to sample all parts leaving the facility. Inhaling or coming in contact with beryllium can cause an immune response that can result in an individual becoming sensitized to beryllium, which can then lead to a disease of the lungs called chronic beryllium disease, and possibly lung cancer. Thirty aluminum and thirty stainless steel parts were fabricated on a lathe in the beryllium facility, as well as thirty-two beryllium parts, for the purpose of testing a parts cleaning method that involved the use of ultrasonic cleaners. A cleaning method was created, documented, validated, and approved, to reduce beryllium contamination.

  19. Improvement of Simulation Method in Validation of Software of the Coordinate Measuring Systems

    Science.gov (United States)

    Nieciąg, Halina

    2015-10-01

    Software is used in order to accomplish various tasks at each stage of the functioning of modern measuring systems. Before metrological confirmation of measuring equipment, the system has to be validated. This paper discusses the method for conducting validation studies of a fragment of software to calculate the values of measurands. Due to the number and nature of the variables affecting the coordinate measurement results and the complex character and multi-dimensionality of measurands, the study used the Monte Carlo method of numerical simulation. The article presents an attempt of possible improvement of results obtained by classic Monte Carlo tools. The algorithm LHS (Latin Hypercube Sampling) was implemented as alternative to the simple sampling schema of classic algorithm.

  20. Improvement of Simulation Method in Validation of Software of the Coordinate Measuring Systems

    Directory of Open Access Journals (Sweden)

    Nieciąg Halina

    2015-10-01

    Full Text Available Software is used in order to accomplish various tasks at each stage of the functioning of modern measuring systems. Before metrological confirmation of measuring equipment, the system has to be validated. This paper discusses the method for conducting validation studies of a fragment of software to calculate the values of measurands. Due to the number and nature of the variables affecting the coordinate measurement results and the complex character and multi-dimensionality of measurands, the study used the Monte Carlo method of numerical simulation. The article presents an attempt of possible improvement of results obtained by classic Monte Carlo tools. The algorithm LHS (Latin Hypercube Sampling was implemented as alternative to the simple sampling schema of classic algorithm.

  1. NordVal: A Nordic system for validation of alternative microbiological methods

    DEFF Research Database (Denmark)

    Qvist, Sven

    2007-01-01

    NordVal was created in 1999 by the Nordic Committee of Senior Officials for Food Issues under the Nordic Council of Ministers. The Committee adopted the following objective for NordVal: NordVal evaluates the performance and field of application of alternative microbiological methods. This includes...... analyses of food, water, feed, animal faeces and food environmental samples in the Nordic countries. NordVal is managed by a steering group, which is appointed by the National Food Administrations in Denmark, Finland, Iceland, Norway and Sweden. The background for creation of NordVal was a Danish...... validation system (DanVal) established in 1995 to cope with a need to validate alternative methods to be used in the Danish Salmonella Action Program. The program attracted considerable attention in the other Nordic countries. NordVal has elaborated a number of documents, which describe the requirements...

  2. Development and Validation of HPLC-PDA Assay method of Frangula emodin

    Directory of Open Access Journals (Sweden)

    Deborah Duca

    2016-03-01

    Full Text Available Frangula emodin, (1,3,8-trihydroxy-6-methyl-anthraquinone, is one of the anthraquinone derivatives found abundantly in the roots and bark of a number of plant families traditionally used to treat constipation and haemorrhoids. The present study describes the development and subsequent validation of a specific Assay HPLC method for emodin. The separation was achieved on a Waters Symmetry C18, 4.6 × 250 mm, 5 μm particle size, column at a temperature of 35 °C, with UV detection at 287 and 436 nm. An isocratic elution mode consisting of 0.1% formic acid and 0.01% trifluoroacetic acid as the aqueous mobile phase, and methanol was used. The method was successfully and statistically validated for linearity, range, precision, accuracy, specificity and solution stability.

  3. HPTLC Method Development and Validation of Zolpidem Tartrate in Bulk and Marketed Formulation

    OpenAIRE

    Abhay R. Shirode; Bharti G. Jadhav; Vilasrao J. Kadam

    2015-01-01

    High performance thin layer chromatography (HPTLC) offers many advantages over HPLC. It reduces the cost of analysis as compare to HPLC. The mobile phase consumption per sample is extremely low in HPTLC, hence reducing the acquisition and disposal cost. Considering the cost and suitability of analysis for estimation of zolpidem tartrate in bulk and its marketed formulation, HPTLC method was developed and validated. The Camag HPTLC system, employed with software winCATS (ver.1.4.1.8) was used ...

  4. Potential of accuracy profile for method validation in inductively coupled plasma spectrochemistry

    International Nuclear Information System (INIS)

    Mermet, J.M.; Granier, G.

    2012-01-01

    Method validation is usually performed over a range of concentrations for which analytical criteria must be verified. One important criterion in quantitative analysis is accuracy, i.e. the contribution of both trueness and precision. The study of accuracy over this range is called an accuracy profile and provides experimental tolerance intervals. Comparison with acceptability limits fixed by the end user defines a validity domain. This work describes the computation involved in the building of the tolerance intervals, particularly for the intermediate precision with within-laboratory experiments and for the reproducibility with interlaboratory studies. Computation is based on ISO 5725‐4 and on previously published work. Moreover, the bias uncertainty is also computed to verify the bias contribution to accuracy. The various types of accuracy profile behavior are exemplified with results obtained by using ICP-MS and ICP-AES. This procedure allows the analyst to define unambiguously a validity domain for a given accuracy. However, because the experiments are time-consuming, the accuracy profile method is mainly dedicated to method validation. - Highlights: ► An analytical method is defined by its accuracy, i.e. both trueness and precision. ► The accuracy as a function of an analyte concentration is an accuracy profile. ► Profile basic concepts are explained for trueness and intermediate precision. ► Profile-based tolerance intervals have to be compared with acceptability limits. ► Typical accuracy profiles are given for both ICP-AES and ICP-MS techniques.

  5. Method Development and Validation for UHPLC-MS-MS Determination of Hop Prenylflavonoids in Human Serum

    OpenAIRE

    Yuan, Yang; Qiu, Xi; Nikolic, Dejan; Dahl, Jeffrey H.; van Breemen, Richard B.

    2012-01-01

    Hops (Humulus lupulus L.) are used in the brewing of beer, and hop extracts containing prenylated compounds such as xanthohumol and 8-prenylnaringenin are under investigation as dietary supplements for cancer chemoprevention and for the management of hot flashes in menopausal women. To facilitate clinical studies of hop safety and efficacy, a selective, sensitive, and fast ultra-high pressure liquid chromatography tandem mass spectrometry (UHPLC-MS-MS) method was developed and validated for t...

  6. The Bland-Altman Method Should Not Be Used in Regression Cross-Validation Studies

    Science.gov (United States)

    O'Connor, Daniel P.; Mahar, Matthew T.; Laughlin, Mitzi S.; Jackson, Andrew S.

    2011-01-01

    The purpose of this study was to demonstrate the bias in the Bland-Altman (BA) limits of agreement method when it is used to validate regression models. Data from 1,158 men were used to develop three regression equations to estimate maximum oxygen uptake (R[superscript 2] = 0.40, 0.61, and 0.82, respectively). The equations were evaluated in a…

  7. Development and Validation of a Stability-Indicating LC-UV Method ...

    African Journals Online (AJOL)

    Development and Validation of a Stability-Indicating LC-UV Method for Simultaneous Determination of Ketotifen and Cetirizine in Pharmaceutical Dosage Forms. ... 5 μm) using an isocratic mobile phase that consisted of acetonitrile and 10 mM disodium hydrogen phosphate buffer (pH 6.5) in a ratio of 45:55 % v/v at a flow ...

  8. Validation of the analytical method for sodium dichloroisocyanurate aimed at drinking water disinfection

    International Nuclear Information System (INIS)

    Martinez Alvarez, Luis Octavio; Alejo Cisneros, Pedro; Garcia Pereira, Reynaldo; Campos Valdez, Doraily

    2014-01-01

    Cuba has developed the first effervescent 3.5 mg sodium dichloroisocyanurate tablets as a non-therapeutic active principle. This ingredient releases certain amount of chlorine when dissolved into a litre of water and it can cause adequate disinfection of drinking water ready to be taken after 30 min. Developing and validating an analytical iodometric method applicable to the quality control of effervescent 3.5 mg sodium dichloroisocyanurate tablets

  9. Validation of verbal autopsy methods using hospital medical records: a case study in Vietnam.

    Science.gov (United States)

    Tran, Hong Thi; Nguyen, Hoa Phuong; Walker, Sue M; Hill, Peter S; Rao, Chalapati

    2018-05-18

    Information on causes of death (COD) is crucial for measuring the health outcomes of populations and progress towards the Sustainable Development Goals. In many countries such as Vietnam where the civil registration and vital statistics (CRVS) system is dysfunctional, information on vital events will continue to rely on verbal autopsy (VA) methods. This study assesses the validity of VA methods used in Vietnam, and provides recommendations on methods for implementing VA validation studies in Vietnam. This validation study was conducted on a sample of 670 deaths from a recent VA study in Quang Ninh province. The study covered 116 cases from this sample, which met three inclusion criteria: a) the death occurred within 30 days of discharge after last hospitalisation, and b) medical records (MRs) for the deceased were available from respective hospitals, and c) the medical record mentioned that the patient was terminally ill at discharge. For each death, the underlying cause of death (UCOD) identified from MRs was compared to the UCOD from VA. The validity of VA diagnoses for major causes of death was measured using sensitivity, specificity and positive predictive value (PPV). The sensitivity of VA was at least 75% in identifying some leading CODs such as stroke, road traffic accidents and several site-specific cancers. However, sensitivity was less than 50% for other important causes including ischemic heart disease, chronic obstructive pulmonary diseases, and diabetes. Overall, there was 57% agreement between UCOD from VA and MR, which increased to 76% when multiple causes from VA were compared to UCOD from MR. Our findings suggest that VA is a valid method to ascertain UCOD in contexts such as Vietnam. Furthermore, within cultural contexts in which patients prefer to die at home instead of a healthcare facility, using the available MRs as the gold standard may be meaningful to the extent that recall bias from the interval between last hospital discharge and death

  10. New clinical validation method for automated sphygmomanometer: a proposal by Japan ISO-WG for sphygmomanometer standard.

    Science.gov (United States)

    Shirasaki, Osamu; Asou, Yosuke; Takahashi, Yukio

    2007-12-01

    Owing to fast or stepwise cuff deflation, or measuring at places other than the upper arm, the clinical accuracy of most recent automated sphygmomanometers (auto-BPMs) cannot be validated by one-arm simultaneous comparison, which would be the only accurate validation method based on auscultation. Two main alternative methods are provided by current standards, that is, two-arm simultaneous comparison (method 1) and one-arm sequential comparison (method 2); however, the accuracy of these validation methods might not be sufficient to compensate for the suspicious accuracy in lateral blood pressure (BP) differences (LD) and/or BP variations (BPV) between the device and reference readings. Thus, the Japan ISO-WG for sphygmomanometer standards has been studying a new method that might improve validation accuracy (method 3). The purpose of this study is to determine the appropriateness of method 3 by comparing immunity to LD and BPV with those of the current validation methods (methods 1 and 2). The validation accuracy of the above three methods was assessed in human participants [N=120, 45+/-15.3 years (mean+/-SD)]. An oscillometric automated monitor, Omron HEM-762, was used as the tested device. When compared with the others, methods 1 and 3 showed a smaller intra-individual standard deviation of device error (SD1), suggesting their higher reproducibility of validation. The SD1 by method 2 (P=0.004) significantly correlated with the participant's BP, supporting our hypothesis that the increased SD of device error by method 2 is at least partially caused by essential BPV. Method 3 showed a significantly (P=0.0044) smaller interparticipant SD of device error (SD2), suggesting its higher interparticipant consistency of validation. Among the methods of validation of the clinical accuracy of auto-BPMs, method 3, which showed the highest reproducibility and highest interparticipant consistency, can be proposed as being the most appropriate.

  11. Bridging the Gap Between Validation and Implementation of Non-Animal Veterinary Vaccine Potency Testing Methods

    Directory of Open Access Journals (Sweden)

    Alistair Currie

    2011-11-01

    Full Text Available In recent years, technologically advanced high-throughput techniques have been developed that replace, reduce or refine animal use in vaccine quality control tests. Following validation, these tests are slowly being accepted for use by international regulatory authorities. Because regulatory acceptance itself has not guaranteed that approved humane methods are adopted by manufacturers, various organizations have sought to foster the preferential use of validated non-animal methods by interfacing with industry and regulatory authorities. After noticing this gap between regulation and uptake by industry, we began developing a paradigm that seeks to narrow the gap and quicken implementation of new replacement, refinement or reduction guidance. A systematic analysis of our experience in promoting the transparent implementation of validated non-animal vaccine potency assays has led to the refinement of our paradigmatic process, presented here, by which interested parties can assess the local regulatory acceptance of methods that reduce animal use and integrate them into quality control testing protocols, or ensure the elimination of peripheral barriers to their use, particularly for potency and other tests carried out on production batches.

  12. Bridging the Gap Between Validation and Implementation of Non-Animal Veterinary Vaccine Potency Testing Methods.

    Science.gov (United States)

    Dozier, Samantha; Brown, Jeffrey; Currie, Alistair

    2011-11-29

    In recent years, technologically advanced high-throughput techniques have been developed that replace, reduce or refine animal use in vaccine quality control tests. Following validation, these tests are slowly being accepted for use by international regulatory authorities. Because regulatory acceptance itself has not guaranteed that approved humane methods are adopted by manufacturers, various organizations have sought to foster the preferential use of validated non-animal methods by interfacing with industry and regulatory authorities. After noticing this gap between regulation and uptake by industry, we began developing a paradigm that seeks to narrow the gap and quicken implementation of new replacement, refinement or reduction guidance. A systematic analysis of our experience in promoting the transparent implementation of validated non-animal vaccine potency assays has led to the refinement of our paradigmatic process, presented here, by which interested parties can assess the local regulatory acceptance of methods that reduce animal use and integrate them into quality control testing protocols, or ensure the elimination of peripheral barriers to their use, particularly for potency and other tests carried out on production batches.

  13. Gradient HPLC method development and validation for Simultaneous estimation of Rosiglitazone and Gliclazide.

    Directory of Open Access Journals (Sweden)

    Uttam Singh Baghel

    2012-10-01

    Full Text Available Objective: The aim of present work was to develop a gradient RP-HPLC method for simultaneous analysis of rosiglitazone and gliclazide, in a tablet dosage form. Method: Chromatographic system was optimized using a hypersil C18 (250mm x 4.6mm, 5毺 m column with potassium dihydrogen phosphate (pH-7.0 and acetonitrile in the ratio of 60:40, as mobile phase, at a flow rate of 1.0 ml/min. Detection was carried out at 225 nm by a SPD-20A prominence UV/Vis detector. Result: Rosiglitazone and gliclazide were eluted with retention times of 17.36 and 7.06 min, respectively. Beer’s Lambert ’s Law was obeyed over the concentration ranges of 5 to 70 毺 g/ml and 2 to 12 毺 g/ml for rosiglitazone and gliclazide, respectively. Conclusion: The high recovery and low coefficients of variation confirm the suitability of the method for simultaneous analysis of both drugs in a tablets dosage form. Statistical analysis proves that the method is sensitive and significant for the analysis of rosiglitazone and gliclazide in pure and in pharmaceutical dosage form without any interference from the excipients. The method was validated in accordance with ICH guidelines. Validation revealed the method is specific, rapid, accurate, precise, reliable, and reproducible.

  14. Validation of a Smartphone Image-Based Dietary Assessment Method for Pregnant Women

    Directory of Open Access Journals (Sweden)

    Amy M. Ashman

    2017-01-01

    Full Text Available Image-based dietary records could lower participant burden associated with traditional prospective methods of dietary assessment. They have been used in children, adolescents and adults, but have not been evaluated in pregnant women. The current study evaluated relative validity of the DietBytes image-based dietary assessment method for assessing energy and nutrient intakes. Pregnant women collected image-based dietary records (via a smartphone application of all food, drinks and supplements consumed over three non-consecutive days. Intakes from the image-based method were compared to intakes collected from three 24-h recalls, taken on random days; once per week, in the weeks following the image-based record. Data were analyzed using nutrient analysis software. Agreement between methods was ascertained using Pearson correlations and Bland-Altman plots. Twenty-five women (27 recruited, one withdrew, one incomplete, median age 29 years, 15 primiparas, eight Aboriginal Australians, completed image-based records for analysis. Significant correlations between the two methods were observed for energy, macronutrients and fiber (r = 0.58–0.84, all p < 0.05, and for micronutrients both including (r = 0.47–0.94, all p < 0.05 and excluding (r = 0.40–0.85, all p < 0.05 supplements in the analysis. Bland-Altman plots confirmed acceptable agreement with no systematic bias. The DietBytes method demonstrated acceptable relative validity for assessment of nutrient intakes of pregnant women.

  15. Validation of the Nuclear Design Method for MOX Fuel Loaded LWR Cores

    International Nuclear Information System (INIS)

    Saji, E.; Inoue, Y.; Mori, M.; Ushio, T.

    2001-01-01

    The actual batch loading of mixed-oxide (MOX) fuel in light water reactors (LWRs) is now ready to start in Japan. One of the efforts that have been devoted to realizing this batch loading has been validation of the nuclear design methods calculating the MOX-fuel-loaded LWR core characteristics. This paper summarizes the validation work for the applicability of the CASMO-4/SIMULATE-3 in-core fuel management code system to MOX-fuel-loaded LWR cores. This code system is widely used by a number of electric power companies for the core management of their commercial LWRs. The validation work was performed for both boiling water reactor (BWR) and pressurized water reactor (PWR) applications. Each validation consists of two parts: analyses of critical experiments and core tracking calculations of operating plants. For the critical experiments, we have chosen a series of experiments known as the VENUS International Program (VIP), which was performed at the SCK/CEN MOL laboratory in Belgium. VIP consists of both BWR and PWR fuel assembly configurations. As for the core tracking calculations, the operating data of MOX-fuel-loaded BWR and PWR cores in Europe have been utilized

  16. Optimization and validation of spectrophotometric methods for determination of finasteride in dosage and biological forms

    Science.gov (United States)

    Amin, Alaa S.; Kassem, Mohammed A.

    2012-01-01

    Aim and Background: Three simple, accurate and sensitive spectrophotometric methods for the determination of finasteride in pure, dosage and biological forms, and in the presence of its oxidative degradates were developed. Materials and Methods: These methods are indirect, involve the addition of excess oxidant potassium permanganate for method A; cerric sulfate [Ce(SO4)2] for methods B; and N-bromosuccinimide (NBS) for method C of known concentration in acid medium to finasteride, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of methylene blue for method A, chromotrope 2R for method B, and amaranth for method C at a suitable maximum wavelength, λmax: 663, 528, and 520 nm, for the three methods, respectively. The reaction conditions for each method were optimized. Results: Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.12–3.84 μg mL–1 for method A, and 0.12–3.28 μg mL–1 for method B and 0.14 – 3.56 μg mL–1 for method C. The apparent molar absorptivity, Sandell sensitivity, detection and quantification limits were evaluated. The stoichiometric ratio between the finasteride and the oxidant was estimated. The validity of the proposed methods was tested by analyzing dosage forms and biological samples containing finasteride with relative standard deviation ≤ 0.95. Conclusion: The proposed methods could successfully determine the studied drug with varying excess of its oxidative degradation products, with recovery between 99.0 and 101.4, 99.2 and 101.6, and 99.6 and 101.0% for methods A, B, and C, respectively. PMID:23781478

  17. 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.

  18. Optimisation and validation of methods to assess single nucleotide polymorphisms (SNPs) in archival histological material

    DEFF Research Database (Denmark)

    Andreassen, C N; Sørensen, Flemming Brandt; Overgaard

    2004-01-01

    only archival specimens are available. This study was conducted to validate protocols optimised for assessment of SNPs based on paraffin embedded, formalin fixed tissue samples.PATIENTS AND METHODS: In 137 breast cancer patients, three TGFB1 SNPs were assessed based on archival histological specimens...... precipitation).RESULTS: Assessment of SNPs based on archival histological material is encumbered by a number of obstacles and pitfalls. However, these can be widely overcome by careful optimisation of the methods used for sample selection, DNA extraction and PCR. Within 130 samples that fulfil the criteria...

  19. Validation of a method to determine methylmercury in fish tissues using gas chromatography

    International Nuclear Information System (INIS)

    Vega Bolannos, Luisa O.; Arias Verdes, Jose A.; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L.

    2000-01-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%

  20. A validated HPTLC method for estimation of moxifloxacin hydrochloride in tablets.

    Science.gov (United States)

    Dhillon, Vandana; Chaudhary, Alok Kumar

    2010-10-01

    A simple HPTLC method having high accuracy, precision and reproducibility was developed for the routine estimation of moxifloxacin hydrochloride in the tablets available in market and was validated for various parameters according to ICH guidelines. moxifloxacin hydrochloride was estimated at 292 nm by densitometry using Silica gel 60 F254 as stationary phase and a premix of methylene chloride: methanol: strong ammonia solution and acetonitrile (10:10:5:10) as mobile phase. Method was found linear in a range of 9-54 nanograms with a correlation coefficient >0.99. The regression equation was: AUC = 65.57 × (Amount in nanograms) + 163 (r(2) = 0.9908).

  1. Lodenafil carbonate tablets: optimization and validation of a capillary zone electrophoresis method

    OpenAIRE

    Codevilla, Cristiane F; Ferreira, Pâmela Cristina L; Sangoi, Maximiliano S; Fröehlich, Pedro Eduardo; Bergold, Ana Maria

    2012-01-01

    A simple capillary zone electrophoresis (CZE) method was developed and validated for the analysis of lodenafil carbonate in tablets. Response surface methodology was used for optimization of the pH and concentration of the buffer, applied voltage and temperature. The method employed 50 mmol L-1 borate buffer at pH 10 as background electrolyte with an applied voltage of 15 kV. The separation was carried out in a fused-silica capillary maintained at 32.5 ºC and the detection wavelength was 214 ...

  2. Validation of the k0 standardization method in neutron activation analysis

    International Nuclear Information System (INIS)

    Kubesova, Marie

    2009-01-01

    The goal of this work was to validate the k 0 standardization method in neutron activation analysis for use by the Nuclear Physics Institute's NAA Laboratory. The precision and accuracy of the method were examined by using two types of reference materials: the one type comprised a set of synthetic materials and served to check the implementation of k 0 standardization, the other type consisted of matrix NIST SRMs comprising various different matrices. In general, a good agreement was obtained between the results of this work and the certified values, giving evidence of the accuracy of our results. In addition, the limits were evaluated for 61 elements

  3. Fibrin Clots Are Equilibrium Polymers That Can Be Remodeled Without Proteolytic Digestion

    OpenAIRE

    Chernysh, Irina N.; Nagaswami, Chandrasekaran; Purohit, Prashant K.; Weisel, John W.

    2012-01-01

    Fibrin polymerization is a necessary part of hemostasis but clots can obstruct blood vessels and cause heart attacks and strokes. The polymerization reactions are specific and controlled, involving strong knob-into-hole interactions to convert soluble fibrinogen into insoluble fibrin. It has long been assumed that clots and thrombi are stable structures until proteolytic digestion. On the contrary, using the technique of fluorescence recovery after photobleaching, we demonstrate here that the...

  4. Diagnosis of hemoparasitosis trough the spread-smear technique using a drop of blood clot

    OpenAIRE

    Neusa Saltiél Stobbe; Eunice Leonora Chaplin; Maria das Graças de Souza Paiva; Nilton Rogério Santos Silva; Flávio A. Pacheco Araújo; Elinor Fortes

    1992-01-01

    The spread-smear technique using a drop of blood clot and stained by diluted and undimitcd Giemsa stain was evaluated for the search of blood cell types and recognition of Babesia bovis, Babesia bigemina and Anaplasma marginale hemoparasites. The blood clot samples were taken from a 6 month-old calf experimentally inoculated with the blood from a Cattle Tick Fever carrier. The Technique was sumitable for the observation of different blood cells and for the recognition of the hemoparasites.

  5. Reliability and validity of a brief method to assess nociceptive flexion reflex (NFR) threshold.

    Science.gov (United States)

    Rhudy, Jamie L; France, Christopher R

    2011-07-01

    The nociceptive flexion reflex (NFR) is a physiological tool to study spinal nociception. However, NFR assessment can take several minutes and expose participants to repeated suprathreshold stimulations. The 4 studies reported here assessed the reliability and validity of a brief method to assess NFR threshold that uses a single ascending series of stimulations (Peak 1 NFR), by comparing it to a well-validated method that uses 3 ascending/descending staircases of stimulations (Staircase NFR). Correlations between the NFR definitions were high, were on par with test-retest correlations of Staircase NFR, and were not affected by participant sex or chronic pain status. Results also indicated the test-retest reliabilities for the 2 definitions were similar. Using larger stimulus increments (4 mAs) to assess Peak 1 NFR tended to result in higher NFR threshold estimates than using the Staircase NFR definition, whereas smaller stimulus increments (2 mAs) tended to result in lower NFR threshold estimates than the Staircase NFR definition. Neither NFR definition was correlated with anxiety, pain catastrophizing, or anxiety sensitivity. In sum, a single ascending series of electrical stimulations results in a reliable and valid estimate of NFR threshold. However, caution may be warranted when comparing NFR thresholds across studies that differ in the ascending stimulus increments. This brief method to assess NFR threshold is reliable and valid; therefore, it should be useful to clinical pain researchers interested in quickly assessing inter- and intra-individual differences in spinal nociceptive processes. Copyright © 2011 American Pain Society. Published by Elsevier Inc. All rights reserved.

  6. Pre-validation methods for developing a patient reported outcome instrument

    Directory of Open Access Journals (Sweden)

    Castillo Mayret M

    2011-08-01

    Full Text Available Abstract Background Measures that reflect patients' assessment of their health are of increasing importance as outcome measures in randomised controlled trials. The methodological approach used in the pre-validation development of new instruments (item generation, item reduction and question formatting should be robust and transparent. The totality of the content of existing PRO instruments for a specific condition provides a valuable resource (pool of items that can be utilised to develop new instruments. Such 'top down' approaches are common, but the explicit pre-validation methods are often poorly reported. This paper presents a systematic and generalisable 5-step pre-validation PRO instrument methodology. Methods The method is illustrated using the example of the Aberdeen Glaucoma Questionnaire (AGQ. The five steps are: 1 Generation of a pool of items; 2 Item de-duplication (three phases; 3 Item reduction (two phases; 4 Assessment of the remaining items' content coverage against a pre-existing theoretical framework appropriate to the objectives of the instrument and the target population (e.g. ICF; and 5 qualitative exploration of the target populations' views of the new instrument and the items it contains. Results The AGQ 'item pool' contained 725 items. Three de-duplication phases resulted in reduction of 91, 225 and 48 items respectively. The item reduction phases discarded 70 items and 208 items respectively. The draft AGQ contained 83 items with good content coverage. The qualitative exploration ('think aloud' study resulted in removal of a further 15 items and refinement to the wording of others. The resultant draft AGQ contained 68 items. Conclusions This study presents a novel methodology for developing a PRO instrument, based on three sources: literature reporting what is important to patient; theoretically coherent framework; and patients' experience of completing the instrument. By systematically accounting for all items dropped

  7. Validation of histamine determination Method in yoghurt using High Performance Liquid Chromatography

    Directory of Open Access Journals (Sweden)

    M Jahedinia

    2014-02-01

    Full Text Available Biogenic amines are organic, basic nitrogenous compounds of low molecular weight that are mainly generated by the enzymatic decarboxylation of amino acids by microorganisms. Dairy products are among the foods with the highest amine content. A wide variety of methods and procedures for determination of histamine and biogenic amines have been established. Amongst, HPLC method is considered as reference method. The aim of this study was to validate Reversed Phase HPLC method determination of histamine in yoghurt. The mobile phase consisted of acetonitrile/water (18:88 v/v and the flow rate was set at 0.5 ml/min using isocratic HPLC. Detection was carried out at 254 nm using UV-detector. Calibration curve that was constructed using peak area of standards was linear and value of correlation coefficient (r2 was estimated at 0.998. Good recoveries were observed for histamine under investigation at all spiking levels and average of recoveries was 84%. The RSD% value from repeatability test was found to be %4.4. Limit of detection and limit of quantitation were 0.14 and 0.42 µ/ml, respectively. The results of validation tests showed that the method is reliable and rapid for quantification of histamine in yoghurt.

  8. Validity of a Simple Method for Measuring Force-Velocity-Power Profile in Countermovement Jump.

    Science.gov (United States)

    Jiménez-Reyes, Pedro; Samozino, Pierre; Pareja-Blanco, Fernando; Conceição, Filipe; Cuadrado-Peñafiel, Víctor; González-Badillo, Juan José; Morin, Jean-Benoît

    2017-01-01

    To analyze the reliability and validity of a simple computation method to evaluate force (F), velocity (v), and power (P) output during a countermovement jump (CMJ) suitable for use in field conditions and to verify the validity of this computation method to compute the CMJ force-velocity (F-v) profile (including unloaded and loaded jumps) in trained athletes. Sixteen high-level male sprinters and jumpers performed maximal CMJs under 6 different load conditions (0-87 kg). A force plate sampling at 1000 Hz was used to record vertical ground-reaction force and derive vertical-displacement data during CMJ trials. For each condition, mean F, v, and P of the push-off phase were determined from both force-plate data (reference method) and simple computation measures based on body mass, jump height (from flight time), and push-off distance and used to establish the linear F-v relationship for each individual. Mean absolute bias values were 0.9% (± 1.6%), 4.7% (± 6.2%), 3.7% (± 4.8%), and 5% (± 6.8%) for F, v, P, and slope of the F-v relationship (S Fv ), respectively. Both methods showed high correlations for F-v-profile-related variables (r = .985-.991). Finally, all variables computed from the simple method showed high reliability, with ICC >.980 and CV push-off distance, and jump height are known.

  9. Development and validation of HPLC analytical method for quantitative determination of metronidazole in human plasma

    International Nuclear Information System (INIS)

    Safdar, K.A.; Shyum, S.B.; Usman, S.

    2016-01-01

    The objective of the present study was to develop a simple, rapid and sensitive reversed-phase high performance liquid chromatographic (RP-HPLC) analytical method with UV detection system for the quantitative determination of metronidazole in human plasma. The chromatographic separation was performed by using C18 RP column (250mm X 4.6mm, 5 meu m) as stationary phase and 0.01M potassium dihydrogen phosphate buffered at pH 3.0 and acetonitrile (83:17, v/v) as mobile phase at flow rate of 1.0 ml/min. The UV detection was carried out at 320nm. The method was validated as per the US FDA guideline for bioanalytical method validation and was found to be selective without interferences from mobile phase components, impurities and biological matrix. The method found to be linear over the concentration range of 0.2812 meu g/ml to 18.0 meu g/ml (r2 = 0.9987) with adequate level of accuracy and precision. The samples were found to be stable under various recommended laboratory and storage conditions. Therefore, the method can be used with adequate level of confidence and assurance for bioavailability, bioequivalence and other pharmacokinetic studies of metronidazole in human. (author)

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

    Directory of Open Access Journals (Sweden)

    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.

  11. Validation and Recommendation of Methods to Measure Biogas Production Potential of Animal Manure

    Directory of Open Access Journals (Sweden)

    C. H. Pham

    2013-06-01

    Full Text Available In developing countries, biogas energy production is seen as a technology that can provide clean energy in poor regions and reduce pollution caused by animal manure. Laboratories in these countries have little access to advanced gas measuring equipment, which may limit research aimed at improving local adapted biogas production. They may also be unable to produce valid estimates of an international standard that can be used for articles published in international peer-reviewed science journals. This study tested and validated methods for measuring total biogas and methane (CH4 production using batch fermentation and for characterizing the biomass. The biochemical methane potential (BMP (CH4 NL kg−1 VS of pig manure, cow manure and cellulose determined with the Moller and VDI methods was not significantly different in this test (p>0.05. The biodegradability using a ratio of BMP and theoretical BMP (TBMP was slightly higher using the Hansen method, but differences were not significant. Degradation rate assessed by methane formation rate showed wide variation within the batch method tested. The first-order kinetics constant k for the cumulative methane production curve was highest when two animal manures were fermented using the VDI 4630 method, indicating that this method was able to reach steady conditions in a shorter time, reducing fermentation duration. In precision tests, the repeatability of the relative standard deviation (RSDr for all batch methods was very low (4.8 to 8.1%, while the reproducibility of the relative standard deviation (RSDR varied widely, from 7.3 to 19.8%. In determination of biomethane concentration, the values obtained using the liquid replacement method (LRM were comparable to those obtained using gas chromatography (GC. This indicates that the LRM method could be used to determine biomethane concentration in biogas in laboratories with limited access to GC.

  12. Inter-laboratory validation of an inexpensive streamlined method to measure inorganic arsenic in rice grain.

    Science.gov (United States)

    Chaney, Rufus L; Green, Carrie E; Lehotay, Steven J

    2018-05-04

    With the establishment by CODEX of a 200 ng/g limit of inorganic arsenic (iAs) in polished rice grain, more analyses of iAs will be necessary to ensure compliance in regulatory and trade applications, to assess quality control in commercial rice production, and to conduct research involving iAs in rice crops. Although analytical methods using high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) have been demonstrated for full speciation of As, this expensive and time-consuming approach is excessive when regulations are based only on iAs. We report a streamlined sample preparation and analysis of iAs in powdered rice based on heated extraction with 0.28 M HNO 3 followed by hydride generation (HG) under control of acidity and other simple conditions. Analysis of iAs is then conducted using flow-injection HG and inexpensive ICP-atomic emission spectroscopy (AES) or other detection means. A key innovation compared with previous methods was to increase the acidity of the reagent solution with 4 M HCl (prior to reduction of As 5+ to As 3+ ), which minimized interferences from dimethylarsinic acid. An inter-laboratory method validation was conducted among 12 laboratories worldwide in the analysis of six shared blind duplicates and a NIST Standard Reference Material involving different types of rice and iAs levels. Also, four laboratories used the standard HPLC-ICP-MS method to analyze the samples. The results between the methods were not significantly different, and the Horwitz ratio averaged 0.52 for the new method, which meets official method validation criteria. Thus, the simpler, more versatile, and less expensive method may be used by laboratories for several purposes to accurately determine iAs in rice grain. Graphical abstract Comparison of iAs results from new and FDA methods.

  13. Validity of a manual soft tissue profile prediction method following mandibular setback osteotomy.

    Science.gov (United States)

    Kolokitha, Olga-Elpis

    2007-10-01

    The aim of this study was to determine the validity of a manual cephalometric method used for predicting the post-operative soft tissue profiles of patients who underwent mandibular setback surgery and compare it to a computerized cephalometric prediction method (Dentofacial Planner). Lateral cephalograms of 18 adults with mandibular prognathism taken at the end of pre-surgical orthodontics and approximately one year after surgery were used. To test the validity of the manual method the prediction tracings were compared to the actual post-operative tracings. The Dentofacial Planner software was used to develop the computerized post-surgical prediction tracings. Both manual and computerized prediction printouts were analyzed by using the cephalometric system PORDIOS. Statistical analysis was performed by means of t-test. Comparison between manual prediction tracings and the actual post-operative profile showed that the manual method results in more convex soft tissue profiles; the upper lip was found in a more prominent position, upper lip thickness was increased and, the mandible and lower lip were found in a less posterior position than that of the actual profiles. Comparison between computerized and manual prediction methods showed that in the manual method upper lip thickness was increased, the upper lip was found in a more anterior position and the lower anterior facial height was increased as compared to the computerized prediction method. Cephalometric simulation of post-operative soft tissue profile following orthodontic-surgical management of mandibular prognathism imposes certain limitations related to the methods implied. However, both manual and computerized prediction methods remain a useful tool for patient communication.

  14. A gradient-based method for segmenting FDG-PET images: methodology and validation

    International Nuclear Information System (INIS)

    Geets, Xavier; Lee, John A.; Gregoire, Vincent; Bol, Anne; Lonneux, Max

    2007-01-01

    A new gradient-based method for segmenting FDG-PET images is described and validated. The proposed method relies on the watershed transform and hierarchical cluster analysis. To allow a better estimation of the gradient intensity, iteratively reconstructed images were first denoised and deblurred with an edge-preserving filter and a constrained iterative deconvolution algorithm. Validation was first performed on computer-generated 3D phantoms containing spheres, then on a real cylindrical Lucite phantom containing spheres of different volumes ranging from 2.1 to 92.9 ml. Moreover, laryngeal tumours from seven patients were segmented on PET images acquired before laryngectomy by the gradient-based method and the thresholding method based on the source-to-background ratio developed by Daisne (Radiother Oncol 2003;69:247-50). For the spheres, the calculated volumes and radii were compared with the known values; for laryngeal tumours, the volumes were compared with the macroscopic specimens. Volume mismatches were also analysed. On computer-generated phantoms, the deconvolution algorithm decreased the mis-estimate of volumes and radii. For the Lucite phantom, the gradient-based method led to a slight underestimation of sphere volumes (by 10-20%), corresponding to negligible radius differences (0.5-1.1 mm); for laryngeal tumours, the segmented volumes by the gradient-based method agreed with those delineated on the macroscopic specimens, whereas the threshold-based method overestimated the true volume by 68% (p = 0.014). Lastly, macroscopic laryngeal specimens were totally encompassed by neither the threshold-based nor the gradient-based volumes. The gradient-based segmentation method applied on denoised and deblurred images proved to be more accurate than the source-to-background ratio method. (orig.)

  15. The application of large amplitude oscillatory stress in a study of fully formed fibrin clots

    Science.gov (United States)

    Lamer, T. F.; Thomas, B. R.; Curtis, D. J.; Badiei, N.; Williams, P. R.; Hawkins, K.

    2017-12-01

    The suitability of controlled stress large amplitude oscillatory shear (LAOStress) for the characterisation of the nonlinear viscoelastic properties of fully formed fibrin clots is investigated. Capturing the rich nonlinear viscoelastic behaviour of the fibrin network is important for understanding the structural behaviour of clots formed in blood vessels which are exposed to a wide range of shear stresses. We report, for the first time, that artefacts due to ringing exist in both the sample stress and strain waveforms of a LAOStress measurement which will lead to errors in the calculation of nonlinear viscoelastic properties. The process of smoothing the waveforms eliminates these artefacts whilst retaining essential rheological information. Furthermore, we demonstrate the potential of LAOStress for characterising the nonlinear viscoelastic properties of fibrin clots in response to incremental increases of applied stress up to the point of fracture. Alternating LAOStress and small amplitude oscillatory shear measurements provide detailed information of reversible and irreversible structural changes of the fibrin clot as a consequence of elevated levels of stress. We relate these findings to previous studies involving large scale deformations of fibrin clots. The LAOStress technique may provide useful information to help understand why some blood clots formed in vessels are stable (such as in deep vein thrombosis) and others break off (leading to a life threatening pulmonary embolism).

  16. Mechanical Stability and Fibrinolytic Resistance of Clots Containing Fibrin, DNA, and Histones*

    Science.gov (United States)

    Longstaff, Colin; Varjú, Imre; Sótonyi, Péter; Szabó, László; Krumrey, Michael; Hoell, Armin; Bóta, Attila; Varga, Zoltán; Komorowicz, Erzsébet; Kolev, Krasimir

    2013-01-01

    Neutrophil extracellular traps are networks of DNA and associated proteins produced by nucleosome release from activated neutrophils in response to infection stimuli and have recently been identified as key mediators between innate immunity, inflammation, and hemostasis. The interaction of DNA and histones with a number of hemostatic factors has been shown to promote clotting and is associated with increased thrombosis, but little is known about the effects of DNA and histones on the regulation of fibrin stability and fibrinolysis. Here we demonstrate that the addition of histone-DNA complexes to fibrin results in thicker fibers (increase in median diameter from 84 to 123 nm according to scanning electron microscopy data) accompanied by improved stability and rigidity (the critical shear stress causing loss of fibrin viscosity increases from 150 to 376 Pa whereas the storage modulus of the gel increases from 62 to 82 pascals according to oscillation rheometric data). The effects of DNA and histones alone are subtle and suggest that histones affect clot structure whereas DNA changes the way clots are lysed. The combination of histones + DNA significantly prolongs clot lysis. Isothermal titration and confocal microscopy studies suggest that histones and DNA bind large fibrin degradation products with 191 and 136 nm dissociation constants, respectively, interactions that inhibit clot lysis. Heparin, which is known to interfere with the formation of neutrophil extracellular traps, appears to prolong lysis time at a concentration favoring ternary histone-DNA-heparin complex formation, and DNase effectively promotes clot lysis in combination with tissue plasminogen activator. PMID:23293023

  17. Using deuterated PAH amendments to validate chemical extraction methods to predict PAH bioavailability in soils

    International Nuclear Information System (INIS)

    Gomez-Eyles, Jose L.; Collins, Chris D.; Hodson, Mark E.

    2011-01-01

    Validating chemical methods to predict bioavailable fractions of polycyclic aromatic hydrocarbons (PAHs) by comparison with accumulation bioassays is problematic. Concentrations accumulated in soil organisms not only depend on the bioavailable fraction but also on contaminant properties. A historically contaminated soil was freshly spiked with deuterated PAHs (dPAHs). dPAHs have a similar fate to their respective undeuterated analogues, so chemical methods that give good indications of bioavailability should extract the fresh more readily available dPAHs and historic more recalcitrant PAHs in similar proportions to those in which they are accumulated in the tissues of test organisms. Cyclodextrin and butanol extractions predicted the bioavailable fraction for earthworms (Eisenia fetida) and plants (Lolium multiflorum) better than the exhaustive extraction. The PAHs accumulated by earthworms had a larger dPAH:PAH ratio than that predicted by chemical methods. The isotope ratio method described here provides an effective way of evaluating other chemical methods to predict bioavailability. - Research highlights: → Isotope ratios can be used to evaluate chemical methods to predict bioavailability. → Chemical methods predicted bioavailability better than exhaustive extractions. → Bioavailability to earthworms was still far from that predicted by chemical methods. - A novel method using isotope ratios to assess the ability of chemical methods to predict PAH bioavailability to soil biota.

  18. Using deuterated PAH amendments to validate chemical extraction methods to predict PAH bioavailability in soils

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Eyles, Jose L., E-mail: j.l.gomezeyles@reading.ac.uk [University of Reading, School of Human and Environmental Sciences, Soil Research Centre, Reading, RG6 6DW Berkshire (United Kingdom); Collins, Chris D.; Hodson, Mark E. [University of Reading, School of Human and Environmental Sciences, Soil Research Centre, Reading, RG6 6DW Berkshire (United Kingdom)

    2011-04-15

    Validating chemical methods to predict bioavailable fractions of polycyclic aromatic hydrocarbons (PAHs) by comparison with accumulation bioassays is problematic. Concentrations accumulated in soil organisms not only depend on the bioavailable fraction but also on contaminant properties. A historically contaminated soil was freshly spiked with deuterated PAHs (dPAHs). dPAHs have a similar fate to their respective undeuterated analogues, so chemical methods that give good indications of bioavailability should extract the fresh more readily available dPAHs and historic more recalcitrant PAHs in similar proportions to those in which they are accumulated in the tissues of test organisms. Cyclodextrin and butanol extractions predicted the bioavailable fraction for earthworms (Eisenia fetida) and plants (Lolium multiflorum) better than the exhaustive extraction. The PAHs accumulated by earthworms had a larger dPAH:PAH ratio than that predicted by chemical methods. The isotope ratio method described here provides an effective way of evaluating other chemical methods to predict bioavailability. - Research highlights: > Isotope ratios can be used to evaluate chemical methods to predict bioavailability. > Chemical methods predicted bioavailability better than exhaustive extractions. > Bioavailability to earthworms was still far from that predicted by chemical methods. - A novel method using isotope ratios to assess the ability of chemical methods to predict PAH bioavailability to soil biota.

  19. The truncated Wigner method for Bose-condensed gases: limits of validity and applications

    International Nuclear Information System (INIS)

    Sinatra, Alice; Lobo, Carlos; Castin, Yvan

    2002-01-01

    We study the truncated Wigner method applied to a weakly interacting spinless Bose-condensed gas which is perturbed away from thermal equilibrium by a time-dependent external potential. The principle of the method is to generate an ensemble of classical fields ψ(r) which samples the Wigner quasi-distribution function of the initial thermal equilibrium density operator of the gas, and then to evolve each classical field with the Gross-Pitaevskii equation. In the first part of the paper we improve the sampling technique over our previous work (Sinatra et al 2000 J. Mod. Opt. 47 2629-44) and we test its accuracy against the exactly solvable model of the ideal Bose gas. In the second part of the paper we investigate the conditions of validity of the truncated Wigner method. For short evolution times it is known that the time-dependent Bogoliubov approximation is valid for almost pure condensates. The requirement that the truncated Wigner method reproduces the Bogoliubov prediction leads to the constraint that the number of field modes in the Wigner simulation must be smaller than the number of particles in the gas. For longer evolution times the nonlinear dynamics of the noncondensed modes of the field plays an important role. To demonstrate this we analyse the case of a three-dimensional spatially homogeneous Bose-condensed gas and we test the ability of the truncated Wigner method to correctly reproduce the Beliaev-Landau damping of an excitation of the condensate. We have identified the mechanism which limits the validity of the truncated Wigner method: the initial ensemble of classical fields, driven by the time-dependent Gross-Pitaevskii equation, thermalizes to a classical field distribution at a temperature T class which is larger than the initial temperature T of the quantum gas. When T class significantly exceeds T a spurious damping is observed in the Wigner simulation. This leads to the second validity condition for the truncated Wigner method, T class - T

  20. Unexpected but Most Welcome: Mixed Methods for the Validation and Revision of the Participatory Evaluation Measurement Instrument

    Science.gov (United States)

    Daigneault, Pierre-Marc; Jacob, Steve

    2014-01-01

    Although combining methods is nothing new, more contributions about why and how to mix methods for validation purposes are needed. This article presents a case of validating the inferences drawn from the Participatory Evaluation Measurement Instrument, an instrument that purports to measure stakeholder participation in evaluation. Although the…

  1. Clashing Validities in the Comparative Method? Balancing In-Depth Understanding and Generalizability in Small-N Policy Studies

    NARCIS (Netherlands)

    van der Heijden, J.

    2013-01-01

    The comparative method receives considerable attention in political science. To some a main advantage of the method is that it allows for both in-depth insights (internal validity), and generalizability beyond the cases studied (external validity). However, others consider internal and external

  2. [Method for evaluating the competence of specialists--the validation of 360-degree-questionnaire].

    Science.gov (United States)

    Nørgaard, Kirsten; Pedersen, Juri; Ravn, Lisbeth; Albrecht-Beste, Elisabeth; Holck, Kim; Fredløv, Maj; Møller, Lars Krag

    2010-04-19

    Assessment of physicians' performance focuses on the quality of their work. The aim of this study was to develop a valid, usable and acceptable multisource feedback assessment tool (MFAT) for hospital consultants. Statements were produced on consultant competencies within non-medical areas like collaboration, professionalism, communication, health promotion, academics and administration. The statements were validated by physicians and later by non-physician professionals after adjustments had been made. In a pilot test, a group of consultants was assessed using the final collection of statements of the MFAT. They received a report with their personal results and subsequently evaluated the assessment method. In total, 66 statements were developed and after validation they were reduced and reformulated to 35. Mean scores for relevance and "easy to understand" of the statements were in the range between "very high degree" and "high degree". In the pilot test, 18 consultants were assessed by themselves, by 141 other physicians and by 125 other professionals in the hospital. About two thirds greatly benefited of the assessment report and half identified areas for personal development. About a third did not want the head of their department to know the assessment results directly; however, two thirds found a potential value in discussing the results with the head. We developed an MFAT for consultants with relevant and understandable statements. A pilot test confirmed that most of the consultants gained from the assessment, but some did not like to share their results with their heads. For these specialists other methods should be used.

  3. An Anatomically Validated Brachial Plexus Contouring Method for Intensity Modulated Radiation Therapy Planning

    International Nuclear Information System (INIS)

    Van de Velde, Joris; Audenaert, Emmanuel; Speleers, Bruno; Vercauteren, Tom; Mulliez, Thomas; Vandemaele, Pieter; Achten, Eric; Kerckaert, Ingrid; D'Herde, Katharina; De Neve, Wilfried; Van Hoof, Tom

    2013-01-01

    Purpose: To develop contouring guidelines for the brachial plexus (BP) using anatomically validated cadaver datasets. Magnetic resonance imaging (MRI) and computed tomography (CT) were used to obtain detailed visualizations of the BP region, with the goal of achieving maximal inclusion of the actual BP in a small contoured volume while also accommodating for anatomic variations. Methods and Materials: CT and MRI were obtained for 8 cadavers positioned for intensity modulated radiation therapy. 3-dimensional reconstructions of soft tissue (from MRI) and bone (from CT) were combined to create 8 separate enhanced CT project files. Dissection of the corresponding cadavers anatomically validated the reconstructions created. Seven enhanced CT project files were then automatically fitted, separately in different regions, to obtain a single dataset of superimposed BP regions that incorporated anatomic variations. From this dataset, improved BP contouring guidelines were developed. These guidelines were then applied to the 7 original CT project files and also to 1 additional file, left out from the superimposing procedure. The percentage of BP inclusion was compared with the published guidelines. Results: The anatomic validation procedure showed a high level of conformity for the BP regions examined between the 3-dimensional reconstructions generated and the dissected counterparts. Accurate and detailed BP contouring guidelines were developed, which provided corresponding guidance for each level in a clinical dataset. An average margin of 4.7 mm around the anatomically validated BP contour is sufficient to accommodate for anatomic variations. Using the new guidelines, 100% inclusion of the BP was achieved, compared with a mean inclusion of 37.75% when published guidelines were applied. Conclusion: Improved guidelines for BP delineation were developed using combined MRI and CT imaging with validation by anatomic dissection

  4. The Validation of AAN Method Used by Rock Sample SRM 2780

    International Nuclear Information System (INIS)

    Rina Mulyaningsih, Th.

    2004-01-01

    AAN methods is a non standard testing method. The testing laboratory must be validate its using method to ensure and confirm that it is suitable with application. The analysis of SRM 2780 Hard rock mine waste with 9 replicates has been done to test the accuracy of AAN methods. The result showed that the elements As, Ba, Mn, V, Zn and Na have good accuration were evaluated against the acceptance criteria for accuracy with confidence level 95 %. The elements As, Co, Sc, Cr, Ba, Sb, Cs, Mn, V, Au, Zn and Na have low relative bias between the analyst's value and the target value. The continued testing must be done to test the accuracy of another certificated elements. (author)

  5. Validated spectrofluorometric method for determination of gemfibrozil in self nanoemulsifying drug delivery systems (SNEDDS)

    Science.gov (United States)

    Sierra Villar, Ana M.; Calpena Campmany, Ana C.; Bellowa, Lyda Halbaut; Trenchs, Monserrat Aróztegui; Naveros, Beatriz Clares

    2013-09-01

    A spectrofluorometric method has been developed and validated for the determination of gemfibrozil. The method is based on the excitation and emission capacities of gemfibrozil with excitation and emission wavelengths of 276 and 304 nm respectively. This method allows de determination of the drug in a self-nanoemulsifying drug delivery system (SNEDDS) for improve its intestinal absorption. Results obtained showed linear relationships with good correlation coefficients (r2 > 0.999) and low limits of detection and quantification (LOD of 0.075 μg mL-1 and LOQ of 0.226 μg mL-1) in the range of 0.2-5 μg mL-1, equally this method showed a good robustness and stability. Thus the amounts of gemfibrozil released from SNEDDS contained in gastro resistant hard gelatine capsules were analysed, and release studies could be performed satisfactorily.

  6. Validated Reverse Phase HPLC Method for the Determination of Impurities in Etoricoxib

    Directory of Open Access Journals (Sweden)

    S. Venugopal

    2011-01-01

    Full Text Available This paper describes the development of reverse phase HPLC method for etoricoxib in the presence of impurities and degradation products generated from the forced degradation studies. The drug substance was subjected to stress conditions of hydrolysis, oxidation, photolysis and thermal degradation. The degradation of etoricoxib was observed under base and oxidation environment. The drug was found stable in other stress conditions studied. Successful separation of the drug from the process related impurities and degradation products were achieved on zorbax SB CN (250 x 4.6 mm 5 μm particle size column using reverse phase HPLC method. The isocratic method employed with a mixture of buffer and acetonitrile in a ratio of 60:40 respectively. Disodium hydrogen orthophosphate (0.02 M is used as buffer and pH adjusted to 7.20 with 1 N sodium hydroxide solution. The HPLC method was developed and validated with respect to linearity, accuracy, precision, specificity and ruggedness.

  7. The Dynamic Similitude Design Method of Thin Walled Structures and Experimental Validation

    Directory of Open Access Journals (Sweden)

    Zhong Luo

    2016-01-01

    Full Text Available For the applicability of dynamic similitude models of thin walled structures, such as engine blades, turbine discs, and cylindrical shells, the dynamic similitude design of typical thin walled structures is investigated. The governing equation of typical thin walled structures is firstly unified, which guides to establishing dynamic scaling laws of typical thin walled structures. Based on the governing equation, geometrically complete scaling law of the typical thin walled structure is derived. In order to determine accurate distorted scaling laws of typical thin walled structures, three principles are proposed and theoretically proved by combining the sensitivity analysis and governing equation. Taking the thin walled annular plate as an example, geometrically complete and distorted scaling laws can be obtained based on the principles of determining dynamic scaling laws. Furthermore, the previous five orders’ accurate distorted scaling laws of thin walled annular plates are presented and numerically validated. Finally, the effectiveness of the similitude design method is validated by experimental annular plates.

  8. Method validation in plasma source optical emission spectroscopy (ICP-OES) - From samples to results

    International Nuclear Information System (INIS)

    Pilon, Fabien; Vielle, Karine; Birolleau, Jean-Claude; Vigneau, Olivier; Labet, Alexandre; Arnal, Nadege; Adam, Christelle; Camilleri, Virginie; Amiel, Jeanine; Granier, Guy; Faure, Joel; Arnaud, Regine; Beres, Andre; Blanchard, Jean-Marc; Boyer-Deslys, Valerie; Broudic, Veronique; Marques, Caroline; Augeray, Celine; Bellefleur, Alexandre; Bienvenu, Philippe; Delteil, Nicole; Boulet, Beatrice; Bourgarit, David; Brennetot, Rene; Fichet, Pascal; Celier, Magali; Chevillotte, Rene; Klelifa, Aline; Fuchs, Gilbert; Le Coq, Gilles; Mermet, Jean-Michel

    2017-01-01

    Even though ICP-OES (Inductively Coupled Plasma - Optical Emission Spectroscopy) is now a routine analysis technique, requirements for measuring processes impose a complete control and mastering of the operating process and of the associated quality management system. The aim of this (collective) book is to guide the analyst during all the measurement validation procedure and to help him to guarantee the mastering of its different steps: administrative and physical management of samples in the laboratory, preparation and treatment of the samples before measuring, qualification and monitoring of the apparatus, instrument setting and calibration strategy, exploitation of results in terms of accuracy, reliability, data covariance (with the practical determination of the accuracy profile). The most recent terminology is used in the book, and numerous examples and illustrations are given in order to a better understanding and to help the elaboration of method validation documents

  9. A Component-Based Modeling and Validation Method for PLC Systems

    Directory of Open Access Journals (Sweden)

    Rui Wang

    2014-05-01

    Full Text Available Programmable logic controllers (PLCs are complex embedded systems that are widely used in industry. This paper presents a component-based modeling and validation method for PLC systems using the behavior-interaction-priority (BIP framework. We designed a general system architecture and a component library for a type of device control system. The control software and hardware of the environment were all modeled as BIP components. System requirements were formalized as monitors. Simulation was carried out to validate the system model. A realistic example from industry of the gates control system was employed to illustrate our strategies. We found a couple of design errors during the simulation, which helped us to improve the dependability of the original systems. The results of experiment demonstrated the effectiveness of our approach.

  10. A Method for Ship Collision Damage and Energy Absorption Analysis and its Validation

    DEFF Research Database (Denmark)

    Zhang, Shengming; Pedersen, Preben Terndrup

    2016-01-01

    -examine this method’s validity andaccuracy for ship collision damage analysis in shipdesign assessments by comprehensive validations withthe experimental results from the public domain. Twentyexperimental tests have been selected, analysed andcompared with the results calculated using the proposedmethod. It can......For design evaluation there is a need for a method whichis fast, practical and yet accurate enough to determine theabsorbed energy and collision damage extent in shipcollision analysis. The most well-known simplifiedempirical approach to collision analysis was madeprobably by Minorsky and its...... limitation is also wellrecognized.The authors have previously developedsimple expressions for the relation between the absorbedenergy and the damaged material volume which take intoaccount the structural arrangements, the materialproperties and the damage modes. The purpose of thepresent paper is to re...

  11. A Method for Ship Collision Damage and Energy Absorption Analysis and its Validation

    DEFF Research Database (Denmark)

    Zhang, Shengming; Pedersen, Preben Terndrup

    2017-01-01

    For design evaluation, there is a need for a method which is fast, practical and yet accurate enough to deter-mine the absorbed energy and collision damage extent in ship collision analysis. The most well-known sim-plified empirical approach to collision analysis was made probably by Minorsky......, and its limitation is alsowell-recognised. The authors have previously developed simple expressions for the relation between theabsorbed energy and the damaged material volume which take into account the structural arrangements,the material properties and the damage modes. The purpose of the present paper...... is to re-examine thismethod’s validity and accuracy for ship collision damage analysis in ship design assessments by compre-hensive validations with experimental results from the public domain. In total, 20 experimental tests havebeen selected, analysed and compared with the results calculated using...

  12. A New Statistical Method to Determine the Degree of Validity of Health Economic Model Outcomes against Empirical Data.

    Science.gov (United States)

    Corro Ramos, Isaac; van Voorn, George A K; Vemer, Pepijn; Feenstra, Talitha L; Al, Maiwenn J

    2017-09-01

    The validation of health economic (HE) model outcomes against empirical data is of key importance. Although statistical testing seems applicable, guidelines for the validation of HE models lack guidance on statistical validation, and actual validation efforts often present subjective judgment of graphs and point estimates. To discuss the applicability of existing validation techniques and to present a new method for quantifying the degrees of validity statistically, which is useful for decision makers. A new Bayesian method is proposed to determine how well HE model outcomes compare with empirical data. Validity is based on a pre-established accuracy interval in which the model outcomes should fall. The method uses the outcomes of a probabilistic sensitivity analysis and results in a posterior distribution around the probability that HE model outcomes can be regarded as valid. We use a published diabetes model (Modelling Integrated Care for Diabetes based on Observational data) to validate the outcome "number of patients who are on dialysis or with end-stage renal disease." Results indicate that a high probability of a valid outcome is associated with relatively wide accuracy intervals. In particular, 25% deviation from the observed outcome implied approximately 60% expected validity. Current practice in HE model validation can be improved by using an alternative method based on assessing whether the model outcomes fit to empirical data at a predefined level of accuracy. This method has the advantage of assessing both model bias and parameter uncertainty and resulting in a quantitative measure of the degree of validity that penalizes models predicting the mean of an outcome correctly but with overly wide credible intervals. Copyright © 2017 International Society for Pharmacoeconomics and Outcomes Research (ISPOR). Published by Elsevier Inc. All rights reserved.

  13. USFDA-GUIDELINE BASED VALIDATION OF TESTING METHOD FOR RIFAMPICIN IN INDONESIAN SERUM SPECIMEN

    Directory of Open Access Journals (Sweden)

    Tri Joko Raharjo

    2010-06-01

    Full Text Available Regarding a new regulation from Indonesia FDA (Badan POM-RI, all new non patent drugs should show bioequivalence with the originator drug prior to registration. Bioequivalence testing (BE-testing has to be performed to the people that represented of population to which the drug to be administrated. BE testing need a valid bio-analytical method for certain drug target and group of population. This research report specific validation of bio-analysis of Rifampicin in Indonesian serum specimen in order to be used for BE testing. The extraction was performed using acetonitrile while the chromatographic separation was accomplished on a RP 18 column (250 × 4.6 mm i.d., 5 µm, with a mobile phase composed of KH2PO4 10 mM-Acetonitrile (40:60, v/v and UV detection was set at 333 nm. The method shown specificity compared to blank serum specimen with retention time of rifampicin at 2.1 min. Lower limit of quantification (LLOQ was 0.06 µg/mL with dynamic range up to 20 µg/mL (R>0.990. Precision of the method was very good with coefficient of variance (CV 0.58; 7.40 and 5.56% for concentration at 0.06, 5, 15 µg/mL, respectively. Accuracies of the method were 3.22; 1.94; 1.90% for concentration 0.06, 5 and 15 µg/mL respectively. The average recoveries were 97.82, 95.50 and 97.31% for concentration of rifampicin 1, 5 and 5 µg/mL, respectively. The method was also shown reliable result on stability test on freezing-thawing, short-term and long-term stability as well as post preparation stability. Validation result shown that the method was ready to be used for Rifampicin BE testing with Indonesian subject.   Keywords: Rifampicin, Validation, USFDA-Guideline

  14. Development and Validation of Spectrophotometric Methods for the Determination of Rasagiline in Pharmaceutical Preparations

    Directory of Open Access Journals (Sweden)

    Serife Evrim Kepekci Tekkeli

    2013-01-01

    Full Text Available This study presents three simple, rapid, and accurate spectrophotometric methods for the determination of Rasagiline (RSG in pharmaceutical preparations. The determination procedures depend on the reaction of RSG with chloranilic acid for method A, tetrachloro-1,4-benzoquinone for method B, and 7,7,8,8-tetracyanoquinodimethane for method C. The colored products were quantitated spectrophotometrically at 524, 535, and 843 nm for methods A, B, and C, respectively. Different variables affecting the reaction were optimized. Linearity ranges of the methods with good correlation coefficients (0.9988–0.9996 were observed as 25–300 µg mL−1, 25–350 µg mL−1, and 50–500 µg mL−1 for methods A, B, and C, respectively. The formation of products takes place through different mechanisms. The sites of interaction were confirmed by elemental analysis using IR and 1H-NMR spectroscopy. The validation of the methods was carried out in terms of specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. No interference was observed from concomitants usually present in dosage forms. The methods were applied successfully to the determination of RSG in pharmaceutical preparations.

  15. Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2013-01-01

    Full Text Available Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue and two sweeteners (Acesulfame-K and Aspartame in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS, is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K and third-derivative curve (for Aspartame and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS, depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1 and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%; recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.

  16. Validation of different spectrophotometric methods for determination of vildagliptin and metformin in binary mixture

    Science.gov (United States)

    Abdel-Ghany, Maha F.; Abdel-Aziz, Omar; Ayad, Miriam F.; Tadros, Mariam M.

    New, simple, specific, accurate, precise and reproducible spectrophotometric methods have been developed and subsequently validated for determination of vildagliptin (VLG) and metformin (MET) in binary mixture. Zero order spectrophotometric method was the first method used for determination of MET in the range of 2-12 μg mL-1 by measuring the absorbance at 237.6 nm. The second method was derivative spectrophotometric technique; utilized for determination of MET at 247.4 nm, in the range of 1-12 μg mL-1. Derivative ratio spectrophotometric method was the third technique; used for determination of VLG in the range of 4-24 μg mL-1 at 265.8 nm. Fourth and fifth methods adopted for determination of VLG in the range of 4-24 μg mL-1; were ratio subtraction and mean centering spectrophotometric methods, respectively. All the results were statistically compared with the reported methods, using one-way analysis of variance (ANOVA). The developed methods were satisfactorily applied to analysis of the investigated drugs and proved to be specific and accurate for quality control of them in pharmaceutical dosage forms.

  17. Validated stability-indicating spectrofluorimetric methods for the determination of ebastine in pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    Eid Manal

    2011-03-01

    Full Text Available Abstract Two sensitive, selective, economic, and validated spectrofluorimetric methods were developed for the determination of ebastine (EBS in pharmaceutical preparations depending on reaction with its tertiary amino group. Method I involves condensation of the drug with mixed anhydrides (citric and acetic anhydrides producing a product with intense fluorescence, which was measured at 496 nm after excitation at 388 nm. Method (IIA describes quantitative fluorescence quenching of eosin upon addition of the studied drug where the decrease in the fluorescence intensity was directly proportional to the concentration of ebastine; the fluorescence quenching was measured at 553 nm after excitation at 457 nm. This method was extended to (Method IIB to apply first and second derivative synchronous spectrofluorimetric method (FDSFS & SDSFS for the simultaneous analysis of EBS in presence of its alkaline, acidic, and UV degradation products. The proposed methods were successfully applied for the determination of the studied compound in its dosage forms. The results obtained were in good agreement with those obtained by a comparison method. Both methods were utilized to investigate the kinetics of the degradation of the drug.

  18. Development and validation of NIR-chemometric methods for chemical and pharmaceutical characterization of meloxicam tablets.

    Science.gov (United States)

    Tomuta, Ioan; Iovanov, Rares; Bodoki, Ede; Vonica, Loredana

    2014-04-01

    Near-Infrared (NIR) spectroscopy is an important component of a Process Analytical Technology (PAT) toolbox and is a key technology for enabling the rapid analysis of pharmaceutical tablets. The aim of this research work was to develop and validate NIR-chemometric methods not only for the determination of active pharmaceutical ingredients content but also pharmaceutical properties (crushing strength, disintegration time) of meloxicam tablets. The development of the method for active content assay was performed on samples corresponding to 80%, 90%, 100%, 110% and 120% of meloxicam content and the development of the methods for pharmaceutical characterization was performed on samples prepared at seven different compression forces (ranging from 7 to 45 kN) using NIR transmission spectra of intact tablets and PLS as a regression method. The results show that the developed methods have good trueness, precision and accuracy and are appropriate for direct active content assay in tablets (ranging from 12 to 18 mg/tablet) and also for predicting crushing strength and disintegration time of intact meloxicam tablets. The comparative data show that the proposed methods are in good agreement with the reference methods currently used for the characterization of meloxicam tablets (HPLC-UV methods for the assay and European Pharmacopeia methods for determining the crushing strength and disintegration time). The results show the possibility to predict both chemical properties (active content) and physical/pharmaceutical properties (crushing strength and disintegration time) directly, without any sample preparation, from the same NIR transmission spectrum of meloxicam tablets.

  19. Raman fiber-optical method for colon cancer detection: Cross-validation and outlier identification approach

    Science.gov (United States)

    Petersen, D.; Naveed, P.; Ragheb, A.; Niedieker, D.; El-Mashtoly, S. F.; Brechmann, T.; Kötting, C.; Schmiegel, W. H.; Freier, E.; Pox, C.; Gerwert, K.

    2017-06-01

    Endoscopy plays a major role in early recognition of cancer which is not externally accessible and therewith in increasing the survival rate. Raman spectroscopic fiber-optical approaches can help to decrease the impact on the patient, increase objectivity in tissue characterization, reduce expenses and provide a significant time advantage in endoscopy. In gastroenterology an early recognition of malign and precursor lesions is relevant. Instantaneous and precise differentiation between adenomas as precursor lesions for cancer and hyperplastic polyps on the one hand and between high and low-risk alterations on the other hand is important. Raman fiber-optical measurements of colon biopsy samples taken during colonoscopy were carried out during a clinical study, and samples of adenocarcinoma (22), tubular adenomas (141), hyperplastic polyps (79) and normal tissue (101) from 151 patients were analyzed. This allows us to focus on the bioinformatic analysis and to set stage for Raman endoscopic measurements. Since spectral differences between normal and cancerous biopsy samples are small, special care has to be taken in data analysis. Using a leave-one-patient-out cross-validation scheme, three different outlier identification methods were investigated to decrease the influence of systematic errors, like a residual risk in misplacement of the sample and spectral dilution of marker bands (esp. cancerous tissue) and therewith optimize the experimental design. Furthermore other validations methods like leave-one-sample-out and leave-one-spectrum-out cross-validation schemes were compared with leave-one-patient-out cross-validation. High-risk lesions were differentiated from low-risk lesions with a sensitivity of 79%, specificity of 74% and an accuracy of 77%, cancer and normal tissue with a sensitivity of 79%, specificity of 83% and an accuracy of 81%. Additionally applied outlier identification enabled us to improve the recognition of neoplastic biopsy samples.

  20. Raman fiber-optical method for colon cancer detection: Cross-validation and outlier identification approach.

    Science.gov (United States)

    Petersen, D; Naveed, P; Ragheb, A; Niedieker, D; El-Mashtoly, S F; Brechmann, T; Kötting, C; Schmiegel, W H; Freier, E; Pox, C; Gerwert, K

    2017-06-15

    Endoscopy plays a major role in early recognition of cancer which is not externally accessible and therewith in increasing the survival rate. Raman spectroscopic fiber-optical approaches can help to decrease the impact on the patient, increase objectivity in tissue characterization, reduce expenses and provide a significant time advantage in endoscopy. In gastroenterology an early recognition of malign and precursor lesions is relevant. Instantaneous and precise differentiation between adenomas as precursor lesions for cancer and hyperplastic polyps on the one hand and between high and low-risk alterations on the other hand is important. Raman fiber-optical measurements of colon biopsy samples taken during colonoscopy were carried out during a clinical study, and samples of adenocarcinoma (22), tubular adenomas (141), hyperplastic polyps (79) and normal tissue (101) from 151 patients were analyzed. This allows us to focus on the bioinformatic analysis and to set stage for Raman endoscopic measurements. Since spectral differences between normal and cancerous biopsy samples are small, special care has to be taken in data analysis. Using a leave-one-patient-out cross-validation scheme, three different outlier identification methods were investigated to decrease the influence of systematic errors, like a residual risk in misplacement of the sample and spectral dilution of marker bands (esp. cancerous tissue) and therewith optimize the experimental design. Furthermore other validations methods like leave-one-sample-out and leave-one-spectrum-out cross-validation schemes were compared with leave-one-patient-out cross-validation. High-risk lesions were differentiated from low-risk lesions with a sensitivity of 79%, specificity of 74% and an accuracy of 77%, cancer and normal tissue with a sensitivity of 79%, specificity of 83% and an accuracy of 81%. Additionally applied outlier identification enabled us to improve the recognition of neoplastic biopsy samples. Copyright

  1. Validation of a food frequency questionnaire to determine vitamin D intakes using the method of triads.

    Science.gov (United States)

    Weir, R R; Carson, E L; Mulhern, M S; Laird, E; Healy, M; Pourshahidi, L K

    2016-04-01

    Dietary sources of vitamin D (both natural and fortified) are increasingly contributing to consumers' vitamin D intake and status. Therefore, the present study aimed to validate a vitamin D food frequency questionnaire (FFQ) for the assessment of habitual vitamin D intake. A total of 49 apparently healthy consenting adults (aged 18-64 years) from the local community were sampled at the end of winter. Dietary intakes were recorded using a 4-day weighed food record (4d-WFR) and a 17-item FFQ based on foods known to contribute to dietary vitamin D intake. Fasting vitamin D status was quantified by serum 25-hydroxyvitamin D [25(OH)D] using liquid chromatography tandem mass spectrometry. The method of triads was applied using these three measurements to determine the overall validity of the FFQ. Vitamin D intakes from 4d-WFR ranged between 0.42 and 31.65 μg day(-1), whereas intakes determined from the FFQ ranged from 1.03 to 36.08 μg day(-1). Serum 25(OH)D concentrations ranged between 12.89 and 279.00 nmol L(-1). The mean (SD) difference between the FFQ and 4d-WFR was +1.62 ( 3.86). There were strong correlations between the vitamin D intake estimated by the FFQ and that from the 4d-WFR (r = 0.562) and also with serum 25(OH)D concentrations (r = 0.567). Vitamin D intake estimated from the 4d-WFR was also strongly correlated with serum 25(OH)D concentrations (r = 0.411). The overall validity coefficient calculated using the method of triads was high (0.881). The vitamin D FFQ has been validated for use in future studies aiming to assess habitual vitamin D intake. © 2015 The British Dietetic Association Ltd.

  2. Probability of identification: a statistical model for the validation of qualitative botanical identification methods.

    Science.gov (United States)

    LaBudde, Robert A; Harnly, James M

    2012-01-01

    A qualitative botanical identification method (BIM) is an analytical procedure that returns a binary result (1 = Identified, 0 = Not Identified). A BIM may be used by a buyer, manufacturer, or regulator to determine whether a botanical material being tested is the same as the target (desired) material, or whether it contains excessive nontarget (undesirable) material. The report describes the development and validation of studies for a BIM based on the proportion of replicates identified, or probability of identification (POI), as the basic observed statistic. The statistical procedures proposed for data analysis follow closely those of the probability of detection, and harmonize the statistical concepts and parameters between quantitative and qualitative method validation. Use of POI statistics also harmonizes statistical concepts for botanical, microbiological, toxin, and other analyte identification methods that produce binary results. The POI statistical model provides a tool for graphical representation of response curves for qualitative methods, reporting of descriptive statistics, and application of performance requirements. Single collaborator and multicollaborative study examples are given.

  3. Method validation using weighted linear regression models for quantification of UV filters in water samples.

    Science.gov (United States)

    da Silva, Claudia Pereira; Emídio, Elissandro Soares; de Marchi, Mary Rosa Rodrigues

    2015-01-01

    This paper describes the validation of a method consisting of solid-phase extraction followed by gas chromatography-tandem mass spectrometry for the analysis of the ultraviolet (UV) filters benzophenone-3, ethylhexyl salicylate, ethylhexyl methoxycinnamate and octocrylene. The method validation criteria included evaluation of selectivity, analytical curve, trueness, precision, limits of detection and limits of quantification. The non-weighted linear regression model has traditionally been used for calibration, but it is not necessarily the optimal model in all cases. Because the assumption of homoscedasticity was not met for the analytical data in this work, a weighted least squares linear regression was used for the calibration method. The evaluated analytical parameters were satisfactory for the analytes and showed recoveries at four fortification levels between 62% and 107%, with relative standard deviations less than 14%. The detection limits ranged from 7.6 to 24.1 ng L(-1). The proposed method was used to determine the amount of UV filters in water samples from water treatment plants in Araraquara and Jau in São Paulo, Brazil. Copyright © 2014 Elsevier B.V. All rights reserved.

  4. Development and validation of a thin-layer chromatography method for stability studies of naproxen

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, Yaslenis; Suarez Perez, Yania; Garcia Pulpeiro, Oscar; Rodriguez Borges, Tania

    2011-01-01

    The validation of an analytical method was carried out to be applied to the stability studies of the future formulations of naproxen suppositories for infant and adult use. The factors which mostly influenced in the naproxen stability were determined, the major degradation occurred in oxidizing acid medium and by action of light. The possible formation of esters between the free carboxyl group present in naproxen and the glyceryl monoestereate present in the base was identified as one of the degradation paths in the new formulation. The results were satisfactory. A thin-layer chromatography-based method was developed as well as the best chromatographic conditions were selected. GF 254 silica gel plates and ultraviolet developer at 254 nm were employed. Three solvent systems were evaluated of which A made up of glacial acetic: tetrahydrofurane:toluene (3:9:90 v/v/v)allowed adequate resolution between the analyte and the possible degradation products, with detection limit of 1 μg. The use of the suggested method was restricted to the identification of possible degradation products just for qualitative purposes and not as final test. The method proved to be sensitive and selective enough to be applied for the stated objective, according to the validation results

  5. Validation of a UV Spectrometric Method for the Assay of Tolfenamic Acid in Organic Solvents

    Directory of Open Access Journals (Sweden)

    Sofia Ahmed

    2015-01-01

    Full Text Available The present study has been carried out to validate a UV spectrometric method for the assay of tolfenamic acid (TA in organic solvents. TA is insoluble in water; therefore, a total of thirteen commonly used organic solvents have been selected in which the drug is soluble. Fresh stock solutions of TA in each solvent in a concentration of 1 × 10−4 M (2.62 mg% were prepared for the assay. The method has been validated according to the guideline of International Conference on Harmonization and parameters like linearity, range, accuracy, precision, sensitivity, and robustness have been studied. Although the method was found to be efficient for the determination of TA in all solvents on the basis of statistical data 1-octanol, followed by ethanol and methanol, was found to be comparatively better than the other studied solvents. No change in the stock solution stability of TA has been observed in each solvent for 24 hours stored either at room (25±1°C or at refrigerated temperature (2–8°C. A shift in the absorption maxima has been observed for TA in various solvents indicating drug-solvent interactions. The studied method is simple, rapid, economical, accurate, and precise for the assay of TA in different organic solvents.

  6. Validation of Field Methods to Assess Body Fat Percentage in Elite Youth Soccer Players.

    Science.gov (United States)

    Munguia-Izquierdo, Diego; Suarez-Arrones, Luis; Di Salvo, Valter; Paredes-Hernandez, Victor; Alcazar, Julian; Ara, Ignacio; Kreider, Richard; Mendez-Villanueva, Alberto

    2018-05-01

    This study determined the most effective field method for quantifying body fat percentage in male elite youth soccer players and developed prediction equations based on anthropometric variables. Forty-four male elite-standard youth soccer players aged 16.3-18.0 years underwent body fat percentage assessments, including bioelectrical impedance analysis and the calculation of various skinfold-based prediction equations. Dual X-ray absorptiometry provided a criterion measure of body fat percentage. Correlation coefficients, bias, limits of agreement, and differences were used as validity measures, and regression analyses were used to develop soccer-specific prediction equations. The equations from Sarria et al. (1998) and Durnin & Rahaman (1967) reached very large correlations and the lowest biases, and they reached neither the practically worthwhile difference nor the substantial difference between methods. The new youth soccer-specific skinfold equation included a combination of triceps and supraspinale skinfolds. None of the practical methods compared in this study are adequate for estimating body fat percentage in male elite youth soccer players, except for the equations from Sarria et al. (1998) and Durnin & Rahaman (1967). The new youth soccer-specific equation calculated in this investigation is the only field method specifically developed and validated in elite male players, and it shows potentially good predictive power. © Georg Thieme Verlag KG Stuttgart · New York.

  7. Development and validation of Ketorolac Tromethamine in eye drop formulation by RP-HPLC method

    Directory of Open Access Journals (Sweden)

    G. Sunil

    2017-02-01

    Full Text Available A simple, precise and accurate method was developed and validated for analysis of Ketorolac Tromethamine in eye drop formulation. An isocratic HPLC analysis was performed on Kromosil C18 column (150 cm × 4.6 mm × 5 μm. The compound was separated with the mixture of methanol and ammonium dihydrogen phosphate buffer in the ratio of 55:45 V/V, pH 3.0 was adjusted with O-phosphoric acid as the mobile phase at flow of 1.5 mL min−1. UV detection was performed at 314 nm using photo diode array detection. The retention time was found to be 6.01 min. The system suitability parameters such as theoretical plate count, tailing and percentage RSD between six standard injections were within the limit. The method was validated according to ICH guidelines. Calibrations were linear over the concentration range of 50–150 μg mL−1 as indicated by correlation coefficient (r of 0.999. The robustness of the method was evaluated by deliberately altering the chromatographic conditions. The developed method can be applicable for routine quantitative analysis.

  8. 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.

  9. Bridging the Gap Between Validation and Implementation of Non-Animal Veterinary Vaccine Potency Testing Methods

    Science.gov (United States)

    Dozier, Samantha; Brown, Jeffrey; Currie, Alistair

    2011-01-01

    Simple Summary Many vaccines are tested for quality in experiments that require the use of large numbers of animals in procedures that often cause significant pain and distress. Newer technologies have fostered the development of vaccine quality control tests that reduce or eliminate the use of animals, but the availability of these newer methods has not guaranteed their acceptance by regulators or use by manufacturers. We discuss a strategic approach that has been used to assess and ultimately increase the use of non-animal vaccine quality tests in the U.S. and U.K. Abstract In recent years, technologically advanced high-throughput techniques have been developed that replace, reduce or refine animal use in vaccine quality control tests. Following validation, these tests are slowly being accepted for use by international regulatory authorities. Because regulatory acceptance itself has not guaranteed that approved humane methods are adopted by manufacturers, various organizations have sought to foster the preferential use of validated non-animal methods by interfacing with industry and regulatory authorities. After noticing this gap between regulation and uptake by industry, we began developing a paradigm that seeks to narrow the gap and quicken implementation of new replacement, refinement or reduction guidance. A systematic analysis of our experience in promoting the transparent implementation of validated non-animal vaccine potency assays has led to the refinement of our paradigmatic process, presented here, by which interested parties can assess the local regulatory acceptance of methods that reduce animal use and integrate them into quality control testing protocols, or ensure the elimination of peripheral barriers to their use, particularly for potency and other tests carried out on production batches. PMID:26486625

  10. Stability indicating method development and validation of assay method for the estimation of rizatriptan benzoate in tablet

    Directory of Open Access Journals (Sweden)

    Chandrashekhar K. Gadewar

    2017-05-01

    Full Text Available A simple, sensitive, precise and specific high performance liquid chromatography method was developed and validated for the determination of rizatriptan in rizatriptan benzoate tablet. The separation was carried out by using a mobile phase consisting of acetonitrile: pH 3.4 phosphate buffer in ratio of 20:80. The column used was Zorbax SB CN 250 mm × 4.6 mm, 5 μ with a flow rate of 1 ml/min using UV detection at 225 nm. The retention time of rizatriptan and benzoic acid was found to be 4.751 and 8.348 min respectively. A forced degradation study of rizatriptan benzoate in its tablet form was conducted under the condition of hydrolysis, oxidation, thermal and photolysis. Rizatriptan was found to be stable in basic buffer while in acidic buffer was found to be degraded (water bath at 60 °C for 15 min. The detector response of rizatriptan is directly proportional to concentration ranging from 30% to 160% of test concentration i.e. 15.032 to 80.172 mcg/ml. Results of analysis were validated statistically and by recovery studies (mean recovery = 99.44. The result of the study showed that the proposed method is simple, rapid, precise and accurate, which is useful for the routine determination of rizatriptan in pharmaceutical dosage forms.

  11. Determination of methylmercury in marine sediment samples: Method validation and occurrence data

    International Nuclear Information System (INIS)

    Carrasco, Luis; Vassileva, Emilia

    2015-01-01

    Highlights: • A method for MeHg determination at trace level in marine sediments is completely validated. • Validation is performed according to ISO-17025 and Eurachem guidelines. • The extraction efficiency of four sample preparation procedures is evaluated. • The uncertainty budget is used as a tool for evaluation of main uncertainty contributors. • Comparison with independent methods yields good agreement within stated uncertainty. - Abstract: The determination of methylmercury (MeHg) in sediment samples is a difficult task due to the extremely low MeHg/THg (total mercury) ratio and species interconversion. Here, we present the method validation of a cost-effective fit-for-purpose analytical procedure for the measurement of MeHg in sediments, which is based on aqueous phase ethylation, followed by purge and trap and hyphenated gas chromatography–pyrolysis–atomic fluorescence spectrometry (GC–Py–AFS) separation and detection. Four different extraction techniques, namely acid and alkaline leaching followed by solvent extraction and evaporation, microwave-assisted extraction with 2-mercaptoethanol, and acid leaching, solvent extraction and back extraction into sodium thiosulfate, were examined regarding their potential to selectively extract MeHg from estuarine sediment IAEA-405 certified reference material (CRM). The procedure based on acid leaching with HNO 3 /CuSO 4 , solvent extraction and back extraction into Na 2 S 2 O 3 yielded the highest extraction recovery, i.e., 94 ± 3% and offered the possibility to perform the extraction of a large number of samples in a short time, by eliminating the evaporation step. The artifact formation of MeHg was evaluated by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC–ICP–MS), using isotopically enriched Me 201 Hg and 202 Hg and it was found to be nonexistent. A full validation approach in line with ISO 17025 and Eurachem guidelines was followed

  12. Determination of methylmercury in marine sediment samples: Method validation and occurrence data

    Energy Technology Data Exchange (ETDEWEB)

    Carrasco, Luis; Vassileva, Emilia, E-mail: e.vasileva-veleva@iaea.org

    2015-01-01

    Highlights: • A method for MeHg determination at trace level in marine sediments is completely validated. • Validation is performed according to ISO-17025 and Eurachem guidelines. • The extraction efficiency of four sample preparation procedures is evaluated. • The uncertainty budget is used as a tool for evaluation of main uncertainty contributors. • Comparison with independent methods yields good agreement within stated uncertainty. - Abstract: The determination of methylmercury (MeHg) in sediment samples is a difficult task due to the extremely low MeHg/THg (total mercury) ratio and species interconversion. Here, we present the method validation of a cost-effective fit-for-purpose analytical procedure for the measurement of MeHg in sediments, which is based on aqueous phase ethylation, followed by purge and trap and hyphenated gas chromatography–pyrolysis–atomic fluorescence spectrometry (GC–Py–AFS) separation and detection. Four different extraction techniques, namely acid and alkaline leaching followed by solvent extraction and evaporation, microwave-assisted extraction with 2-mercaptoethanol, and acid leaching, solvent extraction and back extraction into sodium thiosulfate, were examined regarding their potential to selectively extract MeHg from estuarine sediment IAEA-405 certified reference material (CRM). The procedure based on acid leaching with HNO{sub 3}/CuSO{sub 4}, solvent extraction and back extraction into Na{sub 2}S{sub 2}O{sub 3} yielded the highest extraction recovery, i.e., 94 ± 3% and offered the possibility to perform the extraction of a large number of samples in a short time, by eliminating the evaporation step. The artifact formation of MeHg was evaluated by high performance liquid chromatography coupled to inductively coupled plasma mass spectrometry (HPLC–ICP–MS), using isotopically enriched Me{sup 201}Hg and {sup 202}Hg and it was found to be nonexistent. A full validation approach in line with ISO 17025 and

  13. Fisk-based criteria to support validation of detection methods for drinking water and air.

    Energy Technology Data Exchange (ETDEWEB)

    MacDonell, M.; Bhattacharyya, M.; Finster, M.; Williams, M.; Picel, K.; Chang, Y.-S.; Peterson, J.; Adeshina, F.; Sonich-Mullin, C.; Environmental Science Division; EPA

    2009-02-18

    This report was prepared to support the validation of analytical methods for threat contaminants under the U.S. Environmental Protection Agency (EPA) National Homeland Security Research Center (NHSRC) program. It is designed to serve as a resource for certain applications of benchmark and fate information for homeland security threat contaminants. The report identifies risk-based criteria from existing health benchmarks for drinking water and air for potential use as validation targets. The focus is on benchmarks for chronic public exposures. The priority sources are standard EPA concentration limits for drinking water and air, along with oral and inhalation toxicity values. Many contaminants identified as homeland security threats to drinking water or air would convert to other chemicals within minutes to hours of being released. For this reason, a fate analysis has been performed to identify potential transformation products and removal half-lives in air and water so appropriate forms can be targeted for detection over time. The risk-based criteria presented in this report to frame method validation are expected to be lower than actual operational targets based on realistic exposures following a release. Note that many target criteria provided in this report are taken from available benchmarks without assessing the underlying toxicological details. That is, although the relevance of the chemical form and analogues are evaluated, the toxicological interpretations and extrapolations conducted by the authoring organizations are not. It is also important to emphasize that such targets in the current analysis are not health-based advisory levels to guide homeland security responses. This integrated evaluation of chronic public benchmarks and contaminant fate has identified more than 200 risk-based criteria as method validation targets across numerous contaminants and fate products in drinking water and air combined. The gap in directly applicable values is

  14. Ecological content validation of the Information Assessment Method for parents (IAM-parent): A mixed methods study.

    Science.gov (United States)

    Bujold, M; El Sherif, R; Bush, P L; Johnson-Lafleur, J; Doray, G; Pluye, P

    2018-02-01

    This mixed methods study content validated the Information Assessment Method for parents (IAM-parent) that allows users to systematically rate and comment on online parenting information. Quantitative data and results: 22,407 IAM ratings were collected; of the initial 32 items, descriptive statistics showed that 10 had low relevance. Qualitative data and results: IAM-based comments were collected, and 20 IAM users were interviewed (maximum variation sample); the qualitative data analysis assessed the representativeness of IAM items, and identified items with problematic wording. Researchers, the program director, and Web editors integrated quantitative and qualitative results, which led to a shorter and clearer IAM-parent. Copyright © 2017 The Authors. Published by Elsevier Ltd.. All rights reserved.

  15. Performance of the Tariff Method: validation of a simple additive algorithm for analysis of verbal autopsies

    Directory of Open Access Journals (Sweden)

    Murray Christopher JL

    2011-08-01

    Full Text Available Abstract Background Verbal autopsies provide valuable information for studying mortality patterns in populations that lack reliable vital registration data. Methods for transforming verbal autopsy results into meaningful information for health workers and policymakers, however, are often costly or complicated to use. We present a simple additive algorithm, the Tariff Method (termed Tariff, which can be used for assigning individual cause of death and for determining cause-specific mortality fractions (CSMFs from verbal autopsy data. Methods Tariff calculates a score, or "tariff," for each cause, for each sign/symptom, across a pool of validated verbal autopsy data. The tariffs are summed for a given response pattern in a verbal autopsy, and this sum (score provides the basis for predicting the cause of death in a dataset. We implemented this algorithm and evaluated the method's predictive ability, both in terms of chance-corrected concordance at the individual cause assignment level and in terms of CSMF accuracy at the population level. The analysis was conducted separately for adult, child, and neonatal verbal autopsies across 500 pairs of train-test validation verbal autopsy data. Results Tariff is capable of outperforming physician-certified verbal autopsy in most cases. In terms of chance-corrected concordance, the method achieves 44.5% in adults, 39% in children, and 23.9% in neonates. CSMF accuracy was 0.745 in adults, 0.709 in children, and 0.679 in neonates. Conclusions Verbal autopsies can be an efficient means of obtaining cause of death data, and Tariff provides an intuitive, reliable method for generating individual cause assignment and CSMFs. The method is transparent and flexible and can be readily implemented by users without training in statistics or computer science.

  16. Development and Validation of Liquid Chromatographic Method for Estimation of Naringin in Nanoformulation

    Directory of Open Access Journals (Sweden)

    Kranti P. Musmade

    2014-01-01

    Full Text Available A simple, precise, accurate, rapid, and sensitive reverse phase high performance liquid chromatography (RP-HPLC method with UV detection has been developed and validated for quantification of naringin (NAR in novel pharmaceutical formulation. NAR is a polyphenolic flavonoid present in most of the citrus plants having variety of pharmacological activities. Method optimization was carried out by considering the various parameters such as effect of pH and column. The analyte was separated by employing a C18 (250.0 × 4.6 mm, 5 μm column at ambient temperature in isocratic conditions using phosphate buffer pH 3.5: acetonitrile (75 : 25% v/v as mobile phase pumped at a flow rate of 1.0 mL/min. UV detection was carried out at 282 nm. The developed method was validated according to ICH guidelines Q2(R1. The method was found to be precise and accurate on statistical evaluation with a linearity range of 0.1 to 20.0 μg/mL for NAR. The intra- and interday precision studies showed good reproducibility with coefficients of variation (CV less than 1.0%. The mean recovery of NAR was found to be 99.33 ± 0.16%. The proposed method was found to be highly accurate, sensitive, and robust. The proposed liquid chromatographic method was successfully employed for the routine analysis of said compound in developed novel nanopharmaceuticals. The presence of excipients did not show any interference on the determination of NAR, indicating method specificity.

  17. Validation of a same-day real-time PCR method for screening of meat and carcass swabs for Salmonella

    DEFF Research Database (Denmark)

    Löfström, Charlotta; Krause, Michael; Josefsen, Mathilde Hartmann

    2009-01-01

    of the published PCR methods for Salmonella have been validated in collaborative studies. This study describes a validation including comparative and collaborative trials, based on the recommendations from the Nordic organization for validation of alternative microbiological methods (NordVal) of a same-day, non....... Partly based on results obtained in this study, the method has obtained NordVal approval for analysis of Salmonella in meat and carcass swabs. The PCR method was transferred to a production laboratory and the performance was compared with the BAX Salmonella test on 39 pork samples artificially...... contaminated with Salmonella. There was no significant difference in the results obtained by the two methods. Conclusion: The real-time PCR method for detection of Salmonella in meat and carcass swabs was validated in comparative and collaborative trials according to NordVal recommendations. The PCR method...

  18. A photographic method to measure food item intake. Validation in geriatric institutions.

    Science.gov (United States)

    Pouyet, Virginie; Cuvelier, Gérard; Benattar, Linda; Giboreau, Agnès

    2015-01-01

    From both a clinical and research perspective, measuring food intake is an important issue in geriatric institutions. However, weighing food in this context can be complex, particularly when the items remaining on a plate (side dish, meat or fish and sauce) need to be weighed separately following consumption. A method based on photography that involves taking photographs after a meal to determine food intake consequently seems to be a good alternative. This method enables the storage of raw data so that unhurried analyses can be performed to distinguish the food items present in the images. Therefore, the aim of this paper was to validate a photographic method to measure food intake in terms of differentiating food item intake in the context of a geriatric institution. Sixty-six elderly residents took part in this study, which was performed in four French nursing homes. Four dishes of standardized portions were offered to the residents during 16 different lunchtimes. Three non-trained assessors then independently estimated both the total and specific food item intakes of the participants using images of their plates taken after the meal (photographic method) and a reference image of one plate taken before the meal. Total food intakes were also recorded by weighing the food. To test the reliability of the photographic method, agreements between different assessors and agreements among various estimates made by the same assessor were evaluated. To test the accuracy and specificity of this method, food intake estimates for the four dishes were compared with the food intakes determined using the weighed food method. To illustrate the added value of the photographic method, food consumption differences between the dishes were explained by investigating the intakes of specific food items. Although they were not specifically trained for this purpose, the results demonstrated that the assessor estimates agreed between assessors and among various estimates made by the same

  19. Development and Validation of New Spectrophotometric Methods to Determine Enrofloxacin in Pharmaceuticals

    Science.gov (United States)

    Rajendraprasad, N.; Basavaiah, K.

    2015-07-01

    Four spectrophotometric methods, based on oxidation with cerium(IV), are investigated and developed to determine EFX in pure form and in dosage forms. The frst and second methods (Method A and method B) are direct, in which after the oxidation of EFX with cerium(IV) in acid medium, the absorbance of reduced and unreacted oxidant is measured at 275 and 320 nm, respectively. In the third (C) and fourth (D) methods after the reaction between EFX and oxidant is ensured to be completed the surplus oxidant is treated with either N-phenylanthranilic acid (NPA) or Alizarin Red S (ARS) dye and the absorbance of the oxidized NPA or ARS is measured at 440 or 420 nm. The methods showed good linearity over the concentration ranges of 0.5-5.0, 1.25-12.5, 10.0-100.0, and 6.0-60.0 μg/ml, for method A, B, C and D, respectively, with apparent molar absorptivity values of 4.42 × 10 4 , 8.7 × 10 3 , 9.31 × 10 2 , and 2.28 × 10 3 l/(mol· cm). The limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values and other validation results have also been reported. The proposed methods are successfully applied to determine EFX in pure form and in dosage forms.

  20. Validation of the intrinsic spatial efficiency method for non cylindrical homogeneous sources using MC simulation

    Energy Technology Data Exchange (ETDEWEB)

    Ortiz-Ramírez, Pablo, E-mail: rapeitor@ug.uchile.cl; Ruiz, Andrés [Departamento de Física, Facultad de Ciencias, Universidad de Chile (Chile)

    2016-07-07

    The Monte Carlo simulation of the gamma spectroscopy systems is a common practice in these days. The most popular softwares to do this are MCNP and Geant4 codes. The intrinsic spatial efficiency method is a general and absolute method to determine the absolute efficiency of a spectroscopy system for any extended sources, but this was only demonstrated experimentally for cylindrical sources. Due to the difficulty that the preparation of sources with any shape represents, the simplest way to do this is by the simulation of the spectroscopy system and the source. In this work we present the validation of the intrinsic spatial efficiency method for sources with different geometries and for photons with an energy of 661.65 keV. In the simulation the matrix effects (the auto-attenuation effect) are not considered, therefore these results are only preliminaries. The MC simulation is carried out using the FLUKA code and the absolute efficiency of the detector is determined using two methods: the statistical count of Full Energy Peak (FEP) area (traditional method) and the intrinsic spatial efficiency method. The obtained results show total agreement between the absolute efficiencies determined by the traditional method and the intrinsic spatial efficiency method. The relative bias is lesser than 1% in all cases.

  1. Validation of analytical method for quality control of B12 Vitamin-10 000 injection

    International Nuclear Information System (INIS)

    Botet Garcia, Martha; Garcia Penna, Caridad Margarita; Troche Concepcion, Yenilen; Cannizares Arencibia, Yanara; Moreno Correoso, Barbara

    2009-01-01

    Analytical method reported by USA Pharmacopeia was validated for quality control of injectable B 1 2 Vitamin (10 000 U) by UV spectrophotometry because this is a simpler and low-cost method allowing quality control of finished product. Calibration curve was graphed at 60 to 140% interval, where it was linear with a correlation coefficient similar to 0, 9999; statistical test for interception and slope was considered non-significant. There was a recovery of 99.7 % in study concentrations interval where the Cochran (G) and Student(t) test were not significant too. Variation coefficient in repetition study was similar to 0.59 % for the 6 assayed replies, whereas in intermediate precision analysis, the Fisher and Student tests were not significant. Analytical method was linear, precise, specific and exact in study concentrations interval

  2. Validation and application of an improved method for the rapid determination of proline in grape berries.

    Science.gov (United States)

    Rienth, Markus; Romieu, Charles; Gregan, Rebecca; Walsh, Caroline; Torregrosa, Laurent; Kelly, Mary T

    2014-04-16

    A rapid and sensitive method is presented for the determination of proline in grape berries. Following acidification with formic acid, proline is derivatized by heating at 100 °C for 15 min with 3% ninhydrin in dimethyl sulfoxide, and the absorbance, which is stable for at least 60 min, is read at 520 nm. The method was statistically validated in the concentration range from 2.5 to 15 mg/L, giving a repeatability and intermediate precision of generally amino acid analyzer. In terms of sample preparation, a simple dilution (5-20-fold) is required, and sugars, primary amino acids, and anthocyanins were demonstrated not to interfere, as the latter are bleached by ninhydrin under the experimental conditions. The method was applied to the study of proline accumulation in the fruits of microvines grown in phytotrons, and it was established that proline accumulation and concentrations closely resemble those of field-grown macrovines.

  3. Validation of a residue method to determine pesticide residues in cucumber by using nuclear techniques

    International Nuclear Information System (INIS)

    Baysoyu, D.; Tiryaki, O.; Secer, E.; Aydin, G.

    2009-01-01

    In this study, a multi-residue method using ethyl acetate for extraction and gel permeation chromatography for clean-up was validated to determine chlorpyrifos, malathion and dichlorvos in cucumber by gas chromatography. For this purpose, homogenized cucumber samples were fortified with pesticides at 0.02 0.2, 0.8 and 1 mg/kg levels. The efficiency and repeatability of the method in extraction and cleanup steps were performed using 1 4C-carbaryl by radioisotope tracer technique. 1 4C-carbaryl recoveries after the extraction and cleanup steps were between 92.63-111.73 % with a repeatability of 4.85% (CV) and 74.83-102.22 % with a repeatability of 7.19% (CV), respectively. The homogeneity of analytical samples and the stability of pesticides during homogenization were determined using radio tracer technique and chromatographic methods, respectively.

  4. A New Validated RP- HPLC Method for the Determination of Nevirapine in Human Plasma

    Directory of Open Access Journals (Sweden)

    C. H. Venkata Kumar

    2010-01-01

    Full Text Available A rapid, selective and sensitive high performance liquid chromatographic method for the estimation of nevirapine in human plasma has been developed. Chromatography was carried out on a Hypersil BDS C18 column using a mixture of ammonium acetate buffer (pH 4.0 ± 0.05 and acetonitrile (85:15 v/v as the mobile phase. The eluents were monitored for the drug by UV detection at 254 nm. Oxcarbazepine was used as an internal standard for this study. The retention times for nevirapine and oxcarbazepine were found to be 7.2 and 14.7 min respectively. The method was found to be linear in the concentration range of 50 ng/mL to 5003.7 ng/mL. The method was validated as per FDA guidelines and was found to be suitable for bioequivalence and pharmacokinetic studies.

  5. Analytical method validation for quality control and the study of the 50 mg Propylthiouracil stability

    International Nuclear Information System (INIS)

    Valdes Bendoyro, Maria Olga; Garcia Penna, Caridad Margarita; Fernandez, Juan Lugones; Garcia Borges, Lisandra; Martinez Espinosa, Vivian

    2010-01-01

    A high-performance liquid chromatography analytical method was developed and validated for the quality control and stability studies of 50 mg Propylthiouracil tablets. Method is based in active principle separation through a 100 RP-18 RP-18 (5 μm) (250 x 4 mm) Lichrospher chromatography with UV detection to 272 nm, using a mobile phase composed by a ungaseous mixture of a 0.025 M buffer solution-monobasic potassium phosphate to pH= 4,6 ad acetonitrile in a 80:20 ratio with a flux speed of 0,5 mL/min. Analytical method was linear, precise, specific and exact in the study concentrations interval

  6. Development and Validation of UV Spectrophotometric Method For Estimation of Dolutegravir Sodium in Tablet Dosage Form

    International Nuclear Information System (INIS)

    Balasaheb, B.G.

    2015-01-01

    A simple, rapid, precise and accurate spectrophotometric method has been developed for quantitative analysis of Dolutegravir sodium in tablet formulations. The initial stock solution of Dolutegravir sodium was prepared in methanol solvent and subsequent dilution was done in water. The standard solution of Dolutegravir sodium in water showed maximum absorption at wavelength 259.80 nm. The drug obeyed Beer-Lamberts law in the concentration range of 5-40 μg/ mL with coefficient of correlation (R"2) was 0.9992. The method was validated as per the ICH guidelines. The developed method can be adopted in routine analysis of Dolutegravir sodium in bulk or tablet dosage form and it involves relatively low cost solvents and no complex extraction techniques. (author)

  7. Method validation and uncertainty evaluation of organically bound tritium analysis in environmental sample.

    Science.gov (United States)

    Huang, Yan-Jun; Zeng, Fan; Zhang, Bing; Chen, Chao-Feng; Qin, Hong-Juan; Wu, Lian-Sheng; Guo, Gui-Yin; Yang, Li-Tao; Shang-Guan, Zhi-Hong

    2014-08-01

    The analytical method for organically bound tritium (OBT) was developed in our laboratory. The optimized operating conditions and parameters were established for sample drying, special combustion, distillation, and measurement on a liquid scintillation spectrometer (LSC). Selected types of OBT samples such as rice, corn, rapeseed, fresh lettuce and pork were analyzed for method validation of recovery rate reproducibility, the minimum detection concentration, and the uncertainty for typical low level environmental sample was evaluated. The combustion water recovery rate of different dried environmental sample was kept at about 80%, the minimum detection concentration of OBT ranged from 0.61 to 0.89 Bq/kg (dry weight), depending on the hydrogen content. It showed that this method is suitable for OBT analysis of environmental sample with stable recovery rate, and the combustion water yield of a sample with weight about 40 g would provide sufficient quantity for measurement on LSC. Copyright © 2014 Elsevier Ltd. All rights reserved.

  8. Fuzzy decision-making: a new method in model selection via various validity criteria

    International Nuclear Information System (INIS)

    Shakouri Ganjavi, H.; Nikravesh, K.

    2001-01-01

    Modeling is considered as the first step in scientific investigations. Several alternative models may be candida ted to express a phenomenon. Scientists use various criteria to select one model between the competing models. Based on the solution of a Fuzzy Decision-Making problem, this paper proposes a new method in model selection. The method enables the scientist to apply all desired validity criteria, systematically by defining a proper Possibility Distribution Function due to each criterion. Finally, minimization of a utility function composed of the Possibility Distribution Functions will determine the best selection. The method is illustrated through a modeling example for the A verage Daily Time Duration of Electrical Energy Consumption in Iran

  9. Methods for validating the performance of wearable motion-sensing devices under controlled conditions

    International Nuclear Information System (INIS)

    Bliley, Kara E; Kaufman, Kenton R; Gilbert, Barry K

    2009-01-01

    This paper presents validation methods for assessing the accuracy and precision of motion-sensing device (i.e. accelerometer) measurements. The main goals of this paper were to assess the accuracy and precision of these measurements against a gold standard, to determine if differences in manufacturing and assembly significantly affected device performance and to determine if measurement differences due to manufacturing and assembly could be corrected by applying certain post-processing techniques to the measurement data during analysis. In this paper, the validation of a posture and activity detector (PAD), a device containing a tri-axial accelerometer, is described. Validation of the PAD devices required the design of two test fixtures: a test fixture to position the device in a known orientation, and a test fixture to rotate the device at known velocities and accelerations. Device measurements were compared to these known orientations and accelerations. Several post-processing techniques were utilized in an attempt to reduce variability in the measurement error among the devices. In conclusion, some of the measurement errors due to the inevitable differences in manufacturing and assembly were significantly improved (p < 0.01) by these post-processing techniques

  10. Experimental methods to validate measures of emotional state and readiness for duty in critical operations

    International Nuclear Information System (INIS)

    Weston, Louise Marie

    2007-01-01

    A recent report on criticality accidents in nuclear facilities indicates that human error played a major role in a significant number of incidents with serious consequences and that some of these human errors may be related to the emotional state of the individual. A pre-shift test to detect a deleterious emotional state could reduce the occurrence of such errors in critical operations. The effectiveness of pre-shift testing is a challenge because of the need to gather predictive data in a relatively short test period and the potential occurrence of learning effects due to a requirement for frequent testing. This report reviews the different types of reliability and validity methods and testing and statistical analysis procedures to validate measures of emotional state. The ultimate value of a validation study depends upon the percentage of human errors in critical operations that are due to the emotional state of the individual. A review of the literature to identify the most promising predictors of emotional state for this application is highly recommended

  11. Development and Validation Dissolution Analytical Method of Nimesulide beta-Cyclodextrin 400 mg Tablet

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Carvalho Pereira

    2016-10-01

    Full Text Available The nimesulide (N-(4-nitro-2-phenoxyphenylmethanesulfonamide belongs to the class of non-steroidal anti-inflammatory drugs (NSAIDs and category II of the biopharmaceutical classification, The complexation of nimesulide with b-cyclodextrin is a pharmacological strategy to increase the solubility of the drug The objective of this study was to develop and validate an analytical methodology for dissolving the nimesulide beta-cyclodextrin 400 mg tablet and meets the guidelines of ANVISA for drug registration purposes. Once developed, the dissolution methodology was validated according to the RE of parameters no.  899/2003. In the development of the method it was noted that the duration of the dissolution test was 60 minutes, the volume and the most suitable dissolution medium was 900 mL of aqueous solution of sodium lauryl sulfate 1% (w/ v. It was also noted that rotation of 100 rpm and the paddle apparatus was the most appropriate to evaluate the dissolution of the drug. Spectrophotometric methodology was used to quantify the percentage of dissolved drug. The wavelength was 390 nm using the quantification. The validation of the methodology, system suitability parameters, specificity/selectivity, linearity, precision, accuracy and robustness were satisfactory and proved that the developed dissolution methodology was duly executed. DOI: http://dx.doi.org/10.17807/orbital.v8i5.827

  12. Validation of a method for assessing resident physicians' quality improvement proposals.

    Science.gov (United States)

    Leenstra, James L; Beckman, Thomas J; Reed, Darcy A; Mundell, William C; Thomas, Kris G; Krajicek, Bryan J; Cha, Stephen S; Kolars, Joseph C; McDonald, Furman S

    2007-09-01

    Residency programs involve trainees in quality improvement (QI) projects to evaluate competency in systems-based practice and practice-based learning and improvement. Valid approaches to assess QI proposals are lacking. We developed an instrument for assessing resident QI proposals--the Quality Improvement Proposal Assessment Tool (QIPAT-7)-and determined its validity and reliability. QIPAT-7 content was initially obtained from a national panel of QI experts. Through an iterative process, the instrument was refined, pilot-tested, and revised. Seven raters used the instrument to assess 45 resident QI proposals. Principal factor analysis was used to explore the dimensionality of instrument scores. Cronbach's alpha and intraclass correlations were calculated to determine internal consistency and interrater reliability, respectively. QIPAT-7 items comprised a single factor (eigenvalue = 3.4) suggesting a single assessment dimension. Interrater reliability for each item (range 0.79 to 0.93) and internal consistency reliability among the items (Cronbach's alpha = 0.87) were high. This method for assessing resident physician QI proposals is supported by content and internal structure validity evidence. QIPAT-7 is a useful tool for assessing resident QI proposals. Future research should determine the reliability of QIPAT-7 scores in other residency and fellowship training programs. Correlations should also be made between assessment scores and criteria for QI proposal success such as implementation of QI proposals, resident scholarly productivity, and improved patient outcomes.

  13. Absolute quantification method and validation of airborne snow crab allergen tropomyosin using tandem mass spectrometry

    International Nuclear Information System (INIS)

    Rahman, Anas M. Abdel; Lopata, Andreas L.; Randell, Edward W.; Helleur, Robert J.

    2010-01-01

    Measuring the levels of the major airborne allergens of snow crab in the workplace is very important in studying the prevalence of crab asthma in workers. Previously, snow crab tropomyosin (SCTM) was identified as the major aeroallergen in crab plants and a unique signature peptide was identified for this protein. The present study advances our knowledge on aeroallergens by developing a method of quantification of airborne SCTM by using isotope dilution mass spectrometry. Liquid chromatography tandem mass spectrometry was developed for separation and analysis of the signature peptides. The tryptic digestion conditions were optimized to accomplish complete digestion. The validity of the method was studied using international conference on harmonization protocol, Where 2-9% for CV (precision) and 101-110% for accuracy, at three different levels of quality control. Recovery of the spiked protein from PTFE and TopTip filters was measured to be 99% and 96%, respectively. To further demonstrate the applicability and the validity of the method for real samples, 45 kg of whole snow crab were processed in an enclosed (simulated) crab processing line and air samples were collected. The levels of SCTM ranged between 0.36-3.92 μg m -3 and 1.70-2.31 μg m -3 for butchering and cooking stations, respectively.

  14. Validation of quantitative method for azoxystrobin residues in green beans and peas.

    Science.gov (United States)

    Abdelraheem, Ehab M H; Hassan, Sayed M; Arief, Mohamed M H; Mohammad, Somaia G

    2015-09-01

    This study presents a method validation for extraction and quantitative analysis of azoxystrobin residues in green beans and peas using HPLC-UV and the results confirmed by GC-MS. The employed method involved initial extraction with acetonitrile after the addition of salts (magnesium sulfate and sodium chloride), followed by a cleanup step by activated neutral carbon. Validation parameters; linearity, matrix effect, LOQ, specificity, trueness and repeatability precision were attained. The spiking levels for the trueness and the precision experiments were (0.1, 0.5, 3 mg/kg). For HPLC-UV analysis, mean recoveries ranged between 83.69% to 91.58% and 81.99% to 107.85% for green beans and peas, respectively. For GC-MS analysis, mean recoveries ranged from 76.29% to 94.56% and 80.77% to 100.91% for green beans and peas, respectively. According to these results, the method has been proven to be efficient for extraction and determination of azoxystrobin residues in green beans and peas. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Experimental results and validation of a method to reconstruct forces on the ITER test blanket modules

    International Nuclear Information System (INIS)

    Zeile, Christian; Maione, Ivan A.

    2015-01-01

    Highlights: • An in operation force measurement system for the ITER EU HCPB TBM has been developed. • The force reconstruction methods are based on strain measurements on the attachment system. • An experimental setup and a corresponding mock-up have been built. • A set of test cases representing ITER relevant excitations has been used for validation. • The influence of modeling errors on the force reconstruction has been investigated. - Abstract: In order to reconstruct forces on the test blanket modules in ITER, two force reconstruction methods, the augmented Kalman filter and a model predictive controller, have been selected and developed to estimate the forces based on strain measurements on the attachment system. A dedicated experimental setup with a corresponding mock-up has been designed and built to validate these methods. A set of test cases has been defined to represent possible excitation of the system. It has been shown that the errors in the estimated forces mainly depend on the accuracy of the identified model used by the algorithms. Furthermore, it has been found that a minimum of 10 strain gauges is necessary to allow for a low error in the reconstructed forces.

  16. A Validated Method for the Quality Control of Andrographis paniculata Preparations.

    Science.gov (United States)

    Karioti, Anastasia; Timoteo, Patricia; Bergonzi, Maria Camilla; Bilia, Anna Rita

    2017-10-01

    Andrographis paniculata is a herbal drug of Asian traditional medicine largely employed for the treatment of several diseases. Recently, it has been introduced in Europe for the prophylactic and symptomatic treatment of common cold and as an ingredient of dietary supplements. The active principles are diterpenes with andrographolide as the main representative. In the present study, an analytical protocol was developed for the determination of the main constituents in the herb and preparations of A. paniculata . Three different extraction protocols (methanol extraction using a modified Soxhlet procedure, maceration under ultrasonication, and decoction) were tested. Ultrasonication achieved the highest content of analytes. HPLC conditions were optimized in terms of solvent mixtures, time course, and temperature. A reversed phase C18 column eluted with a gradient system consisting of acetonitrile and acidified water and including an isocratic step at 30 °C was used. The HPLC method was validated for linearity, limits of quantitation and detection, repeatability, precision, and accuracy. The overall method was validated for precision and accuracy over at least three different concentration levels. Relative standard deviation was less than 1.13%, whereas recovery was between 95.50% and 97.19%. The method also proved to be suitable for the determination of a large number of commercial samples and was proposed to the European Pharmacopoeia for the quality control of Andrographidis herba. Georg Thieme Verlag KG Stuttgart · New York.

  17. Validation of an ultra-fast UPLC-UV method for the separation of antituberculosis tablets.

    Science.gov (United States)

    Nguyen, Dao T-T; Guillarme, Davy; Rudaz, Serge; Veuthey, Jean-Luc

    2008-04-01

    A simple method using ultra performance LC (UPLC) coupled with UV detection was developed and validated for the determination of antituberculosis drugs in combined dosage form, i. e. isoniazid (ISN), pyrazinamide (PYR) and rifampicin (RIF). Drugs were separated on a short column (2.1 mm x 50 mm) packed with 1.7 mum particles, using an elution gradient procedure. At 30 degrees C, less than 2 min was necessary for the complete separation of the three antituberculosis drugs, while the original USP method was performed in 15 min. Further improvements were obtained with the combination of UPLC and high temperature (up to 90 degrees C), namely HT-UPLC, which allows the application of higher mobile phase flow rates. Therefore, the separation of ISN, PYR and RIF was performed in less than 1 min. After validation (selectivity, trueness, precision and accuracy), both methods (UPLC and HT-UPLC) have proven suitable for the routine quality control analysis of antituberculosis drugs in combined dosage form. Additionally, a large number of samples per day can be analysed due to the short analysis times.

  18. Determination of methylmercury in marine biota samples with advanced mercury analyzer: method validation.

    Science.gov (United States)

    Azemard, Sabine; Vassileva, Emilia

    2015-06-01

    In this paper, we present a simple, fast and cost-effective method for determination of methyl mercury (MeHg) in marine samples. All important parameters influencing the sample preparation process were investigated and optimized. Full validation of the method was performed in accordance to the ISO-17025 (ISO/IEC, 2005) and Eurachem guidelines. Blanks, selectivity, working range (0.09-3.0ng), recovery (92-108%), intermediate precision (1.7-4.5%), traceability, limit of detection (0.009ng), limit of quantification (0.045ng) and expanded uncertainty (15%, k=2) were assessed. Estimation of the uncertainty contribution of each parameter and the demonstration of traceability of measurement results was provided as well. Furthermore, the selectivity of the method was studied by analyzing the same sample extracts by advanced mercury analyzer (AMA) and gas chromatography-atomic fluorescence spectrometry (GC-AFS). Additional validation of the proposed procedure was effectuated by participation in the IAEA-461 worldwide inter-laboratory comparison exercises. Copyright © 2014 Elsevier Ltd. All rights reserved.

  19. Validated method for the analysis of goji berry, a rich source of zeaxanthin dipalmitate.

    Science.gov (United States)

    Karioti, Anastasia; Bergonzi, Maria Camilla; Vincieri, Franco F; Bilia, Anna Rita

    2014-12-31

    In the present study an HPLC-DAD method was developed for the determination of the main carotenoid, zeaxanthin dipalmitate, in the fruits of Lycium barbarum. The aim was to develop and optimize an extraction protocol to allow fast, exhaustive, and repeatable extraction, suitable for labile carotenoid content. Use of liquid N2 allowed the grinding of the fruit. A step of ultrasonication with water removed efficiently the polysaccharides and enabled the exhaustive extraction of carotenoids by hexane/acetone 50:50. The assay was fast and simple and permitted the quality control of a large number of commercial samples including fruits, juices, and a jam. The HPLC method was validated according to ICH guidelines and satisfied the requirements. Finally, the overall method was validated for precision (% RSD ranging between 3.81 and 4.13) and accuracy at three concentration levels. The recovery was between 94 and 107% with RSD values <2%, within the acceptable limits, especially if the difficulty of the matrix is taken into consideration.

  20. A Validated RP-HPLC Method for Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    G. Tulja Rani

    2011-01-01

    Full Text Available A simple, fast, precise, selective and accurate RP-HPLC method was developed and validated for the simultaneous determination of atenolol and indapamide from bulk and formulations. Chromatographic separation was achieved isocratically on a Waters C18 column (250×4.6 mm, 5 µ particle size using a mobile phase, methanol and water (adjusted to pH 2.7 with 1% orthophosphoric acid in the ratio of 80:20. The flow rate was 1 mL/min and effluent was detected at 230 nm. The retention time of atenolol and indapamide were 1.766 min and 3.407 min. respectively. Linearity was observed in the concentration range of 12.5-150 µg/mL for atenolol and 0.625-7.5 µg/mL for indapamide. Percent recoveries obtained for both the drugs were 99.74-100.06% and 98.65-99.98% respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method developed can be used for the routine analysis of atenolol and indapamide from their combined dosage form.

  1. Absolute quantification method and validation of airborne snow crab allergen tropomyosin using tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rahman, Anas M. Abdel, E-mail: anasar@mun.ca [Department of Chemistry, Memorial University of Newfoundland, St. John' s, Newfoundland A1B 3X7 (Canada); Lopata, Andreas L. [School of Applied Science, Marine Biomedical Sciences and Health Research Group, RMIT University, Bundoora, 3083 Victoria (Australia); Randell, Edward W. [Department of Laboratory Medicine, Memorial University of Newfoundland, Eastern Health, St. John' s, Newfoundland and Labrador A1B 3V6 (Canada); Helleur, Robert J. [Department of Chemistry, Memorial University of Newfoundland, St. John' s, Newfoundland A1B 3X7 (Canada)

    2010-11-29

    Measuring the levels of the major airborne allergens of snow crab in the workplace is very important in studying the prevalence of crab asthma in workers. Previously, snow crab tropomyosin (SCTM) was identified as the major aeroallergen in crab plants and a unique signature peptide was identified for this protein. The present study advances our knowledge on aeroallergens by developing a method of quantification of airborne SCTM by using isotope dilution mass spectrometry. Liquid chromatography tandem mass spectrometry was developed for separation and analysis of the signature peptides. The tryptic digestion conditions were optimized to accomplish complete digestion. The validity of the method was studied using international conference on harmonization protocol, Where 2-9% for CV (precision) and 101-110% for accuracy, at three different levels of quality control. Recovery of the spiked protein from PTFE and TopTip filters was measured to be 99% and 96%, respectively. To further demonstrate the applicability and the validity of the method for real samples, 45 kg of whole snow crab were processed in an enclosed (simulated) crab processing line and air samples were collected. The levels of SCTM ranged between 0.36-3.92 {mu}g m{sup -3} and 1.70-2.31 {mu}g m{sup -3} for butchering and cooking stations, respectively.

  2. A validated high performance thin layer chromatography method for determination of yohimbine hydrochloride in pharmaceutical preparations.

    Science.gov (United States)

    Badr, Jihan M

    2013-01-01

    Yohimbine is an indole alkaloid used as a promising therapy for erectile dysfunction. A number of methods were reported for the analysis of yohimbine in the bark or in pharmaceutical preparations. In the present work, a simple and sensitive high performance thin layer chromatographic method is developed for determination of yohimbine (occurring as yohimbine hydrochloride) in pharmaceutical preparations and validated according to International Conference of Harmonization (ICH) guidelines. The method employed thin layer chromatography aluminum sheets precoated with silica gel as the stationary phase and the mobile phase consisted of chloroform:methanol:ammonia (97:3:0.2), which gave compact bands of yohimbine hydrochloride. Linear regression data for the calibration curves of standard yohimbine hydrochloride showed a good linear relationship over a concentration range of 80-1000 ng/spot with respect to the area and correlation coefficient (R(2)) was 0.9965. The method was evaluated regarding accuracy, precision, selectivity, and robustness. Limits of detection and quantitation were recorded as 5 and 40 ng/spot, respectively. The proposed method efficiently separated yohimbine hydrochloride from other components even in complex mixture containing powdered plants. The amount of yohimbine hydrochloride ranged from 2.3 to 5.2 mg/tablet or capsule in preparations containing the pure alkaloid, while it varied from zero (0) to 1.5-1.8 mg/capsule in dietary supplements containing powdered yohimbe bark. We concluded that this method employing high performance thin layer chromatography (HPTLC) in quantitative determination of yohimbine hydrochloride in pharmaceutical preparations is efficient, simple, accurate, and validated.

  3. Contribution to the validation of thermal ratchetting prevision methods in metallic structures

    International Nuclear Information System (INIS)

    Rakotovelo, A.M.

    1998-03-01

    This work concerns the steady state assessment in the metallic structures subjected to thermomechanical cyclic loadings in biaxial stress state. The effect of the short time mechanical overloads is also investigated. The first chapter is devoted to a bibliographic research concerning the behaviour of the materials and the structures in the cyclic plasticity. Some works relate to the experimental aspect as well as the numerical one for the steady state assessment of such structures are presented. The experimental part of the study is presented in the second chapter. The experimental device was carried out in order to prescribe tension and torsion forces combined with cyclic thermal loading. Some tests was then carried out, among these tests certain include some overloads in tension or torsion. The last chapter describes the numerical calculations using different models (linear isotropic hardening, linear kinematic hardening and elasto-viscoplastic Chaboche's model) and the application of some simplified methods for the ratchetting assessment in the structures. We have considered two categories of methods. The first one is based on an elastic analysis (Bree's diagram, 3 Sm rule, efficiency rule) and the second one combines elastic analysis and elastoplastic analysis of the first cycle (Gatt's and Taleb's methods). The results of this study have enabled: to validate in the biaxial stress state an expression which takes into account the effect of mechanical short time overloads; to test the performances of considered models to describe the evolution of the structure during the first cycle and to take into account the effect of short time overloads. Among the considered models, the elastoplastic Chaboche's model seems to be the most accurate to describe the structure's behaviour during the first cycles; to validate some simplified methods. Certain methods based only on elastic analysis (Bee's diagram and efficiency rule) seem not suitable for the considered kind of

  4. Validation of quantitative 1H NMR method for the analysis of pharmaceutical formulations

    International Nuclear Information System (INIS)

    Santos, Maiara da S.

    2013-01-01

    The need for effective and reliable quality control in products from pharmaceutical industries renders the analyses of their active ingredients and constituents of great importance. This study presents the theoretical basis of ¹H NMR for quantitative analyses and an example of the method validation according to Resolution RE N. 899 by the Brazilian National Health Surveillance Agency (ANVISA), in which the compound paracetamol was the active ingredient. All evaluated parameters (selectivity, linearity, accuracy, repeatability and robustness) showed satisfactory results. It was concluded that a single NMR measurement provides structural and quantitative information of active components and excipients in the sample. (author)

  5. Analytical Method Development and Validation of Solifenacin in Pharmaceutical Dosage Forms by RP-HPLC

    OpenAIRE

    Shaik, Rihana Parveen; Puttagunta, Srinivasa Babu; Kothapalli Bannoth, Chandrasekar; Challa, Bala Sekhara Reddy

    2014-01-01

    A new, accurate, precise, and robust HPLC method was developed and validated for the determination of solifenacin in tablet dosage form. The chromatographic separation was achieved on an Inertsil ODS 3V C18 (150 mm × 4.6 mm, 5 μm) stationary phase maintained at ambient temperature with a mobile phase combination of monobasic potassium phosphate (pH 3.5) containing 0.1% triethylamine and methanol (gradient mode) at a flow rate of 1.5 mL/min, and the detection was carried out by using UV detect...

  6. Summary of Validation of Multi-Pesticide Methods for Various Pesticide Formulations

    Energy Technology Data Exchange (ETDEWEB)

    Ambrus, A. [Hungarian Food Safety Office, Budapest (Hungary)

    2009-07-15

    The validation of multi-pesticide methods applicable for various types of pesticide formulations is treated. In a worked-out practical example, i.e. lambda cyhalothrin, the theoretical considerations outlined in the General Guidance section are put into practice. GC conditions, selection of an internal standard and criteria for an acceptable repeatability of injections are outlined, followed by sample preparation, calibration, batch analysis and confirmation of results through comparison using different separation columns. Complete sets of data are displayed in tabular form for other pesticide active ingredients and real formulations. (author)

  7. Results of a survey on accident and safety analysis codes, benchmarks, verification and validation methods

    International Nuclear Information System (INIS)

    Lee, A.G.; Wilkin, G.B.

    1995-01-01

    This report is a compilation of the information submitted by AECL, CIAE, JAERI, ORNL and Siemens in response to a need identified at the 'Workshop on R and D Needs' at the IGORR-3 meeting. The survey compiled information on the national standards applied to the Safety Quality Assurance (SQA) programs undertaken by the participants. Information was assembled for the computer codes and nuclear data libraries used in accident and safety analyses for research reactors and the methods used to verify and validate the codes and libraries. Although the survey was not comprehensive, it provides a basis for exchanging information of common interest to the research reactor community

  8. Validation of the LWR-EIR methods for the evaluation of compact beds

    International Nuclear Information System (INIS)

    Foskolos, K.; Grimm, P.; Maeder, C.; Paratte, J.M.

    1983-10-01

    The EIR code system for the calculation of light water reactors is presented and the methods used are briefly described. The application of the system on various types of critical experiments and benchmark problems proves its good precision, even for heterogeneous configurations with strong neutron absorbers like Boral. As the accuracy of the multiplication factor ksub(eff) is always better than 0.5% for normal LWR configurations, this code system is validated for the calculation of such configurations with a safety margin of 1.5% on ksub(eff). (Auth.)

  9. Validation of the EIR LWR calculation methods for criticality assessment of storage pools

    International Nuclear Information System (INIS)

    Grimm, P.; Paratte, J.M.

    1986-11-01

    The EIR code system for the calculation of light water reactors is presented and the methods used are briefly described. The application of the system to various types of critical experiments and benchmark problems proves its good accuracy, even for heterogeneous configurations containing strong neutron absorbers such as Boral. Since the multiplication factor k eff is normally somewhat overpredicted and the spread of the results is small, this code system is validated for the calculation of storage pools, taking into account a safety margins of 1.5% on k eff . (author)

  10. Validated spectophotometric methods for the assay of cinitapride hydrogen tartrate in pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Satyanarayana K.V.V.

    2013-01-01

    Full Text Available Three simple, selective and rapid spectrophotometric methods have been established for the determination of cinitapride hydrogen tartrate (CHT in pharmaceutical tablets. The proposed methods are based on the diazotization of CHT with sodium nitrite and hydrochloric acid, followed by coupling with resorcinol, 1-benzoylacetone and 8-hydroxyquinoline in alkaline medium for methods A, B and C respectively. The formed azo dyes are measured at 442, 465 and 552 nm for methods A, B and C respectively. The parameters that affect the reaction were carefully optimized. Under optimum conditions, Beer’s law is obeyed over the ranges 2.0-32.0, 1.0-24.0 and 1.0-20.0 μg. mL-1 for methods A, B, and C, respectively. The calculated molar absorptivity values are 1.2853 x104, 1.9624 x104 and 3.92 x104 L.mol-1.cm-1 for methods A, B and C, respectively. The results of the proposed procedures were validated statistically according to ICH guidelines. The proposed methods were successfully applied to the determination of CHT in Cintapro tablets without interference from common excipients encountered.

  11. Validity studies among hierarchical methods of cluster analysis using cophenetic correlation coefficient

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, Priscilla R.; Munita, Casimiro S.; Lapolli, André L., E-mail: prii.ramos@gmail.com, E-mail: camunita@ipen.br, E-mail: alapolli@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

    2017-07-01

    The literature presents many methods for partitioning of data base, and is difficult choose which is the most suitable, since the various combinations of methods based on different measures of dissimilarity can lead to different patterns of grouping and false interpretations. Nevertheless, little effort has been expended in evaluating these methods empirically using an archaeological data base. In this way, the objective of this work is make a comparative study of the different cluster analysis methods and identify which is the most appropriate. For this, the study was carried out using a data base of the Archaeometric Studies Group from IPEN-CNEN/SP, in which 45 samples of ceramic fragments from three archaeological sites were analyzed by instrumental neutron activation analysis (INAA) which were determinate the mass fraction of 13 elements (As, Ce, Cr, Eu, Fe, Hf, La, Na, Nd, Sc, Sm, Th, U). The methods used for this study were: single linkage, complete linkage, average linkage, centroid and Ward. The validation was done using the cophenetic correlation coefficient and comparing these values the average linkage method obtained better results. A script of the statistical program R with some functions was created to obtain the cophenetic correlation. By means of these values was possible to choose the most appropriate method to be used in the data base. (author)

  12. Validity studies among hierarchical methods of cluster analysis using cophenetic correlation coefficient

    International Nuclear Information System (INIS)

    Carvalho, Priscilla R.; Munita, Casimiro S.; Lapolli, André L.

    2017-01-01

    The literature presents many methods for partitioning of data base, and is difficult choose which is the most suitable, since the various combinations of methods based on different measures of dissimilarity can lead to different patterns of grouping and false interpretations. Nevertheless, little effort has been expended in evaluating these methods empirically using an archaeological data base. In this way, the objective of this work is make a comparative study of the different cluster analysis methods and identify which is the most appropriate. For this, the study was carried out using a data base of the Archaeometric Studies Group from IPEN-CNEN/SP, in which 45 samples of ceramic fragments from three archaeological sites were analyzed by instrumental neutron activation analysis (INAA) which were determinate the mass fraction of 13 elements (As, Ce, Cr, Eu, Fe, Hf, La, Na, Nd, Sc, Sm, Th, U). The methods used for this study were: single linkage, complete linkage, average linkage, centroid and Ward. The validation was done using the cophenetic correlation coefficient and comparing these values the average linkage method obtained better results. A script of the statistical program R with some functions was created to obtain the cophenetic correlation. By means of these values was possible to choose the most appropriate method to be used in the data base. (author)

  13. Estimating incidence from prevalence in generalised HIV epidemics: methods and validation.

    Directory of Open Access Journals (Sweden)

    Timothy B Hallett

    2008-04-01

    Full Text Available HIV surveillance of generalised epidemics in Africa primarily relies on prevalence at antenatal clinics, but estimates of incidence in the general population would be more useful. Repeated cross-sectional measures of HIV prevalence are now becoming available for general populations in many countries, and we aim to develop and validate methods that use these data to estimate HIV incidence.Two methods were developed that decompose observed changes in prevalence between two serosurveys into the contributions of new infections and mortality. Method 1 uses cohort mortality rates, and method 2 uses information on survival after infection. The performance of these two methods was assessed using simulated data from a mathematical model and actual data from three community-based cohort studies in Africa. Comparison with simulated data indicated that these methods can accurately estimates incidence rates and changes in incidence in a variety of epidemic conditions. Method 1 is simple to implement but relies on locally appropriate mortality data, whilst method 2 can make use of the same survival distribution in a wide range of scenarios. The estimates from both methods are within the 95% confidence intervals of almost all actual measurements of HIV incidence in adults and young people, and the patterns of incidence over age are correctly captured.It is possible to estimate incidence from cross-sectional prevalence data with sufficient accuracy to monitor the HIV epidemic. Although these methods will theoretically work in any context, we have able to test them only in southern and eastern Africa, where HIV epidemics are mature and generalised. The choice of method will depend on the local availability of HIV mortality data.

  14. Ability of Polyphosphate and Nucleic Acids to Trigger Blood Clotting: Some Observations and Caveats

    Science.gov (United States)

    Smith, Stephanie A.; Gajsiewicz, Joshua M.; Morrissey, James H.

    2018-01-01

    Polyphosphate plays several roles in coagulation and inflammation, while extracellular DNA and RNA are implicated in thrombosis and as disease biomarkers. We sought to compare the procoagulant activities of polyphosphate versus DNA or RNA isolated from mammalian cells. In a recent study, we found that much of the procoagulant activity of DNA isolated from mammalian cells using Qiagen kits resisted digestion with nuclease or polyphosphatase, and even resisted boiling in acid. These kits employ spin columns packed with silica, which is highly procoagulant. Indeed, much of the apparent procoagulant activity of cellular DNA isolated with such kits was attributable to silica particles shed by the spin columns. Therefore, silica-based methods for isolating nucleic acids or polyphosphate from mammalian cells are not suitable for studying their procoagulant activities. We now report that polyphosphate readily co-purified with DNA and RNA using several popular isolation methods, including phenol/chloroform extraction. Thus, cell-derived nucleic acids are also subject to contamination with traces of cellular polyphosphate, which can be eliminated by alkaline phosphatase digestion. We further report that long-chain polyphosphate was orders of magnitude more potent than cell-derived DNA (purified via phenol/chloroform extraction) or RNA at triggering clotting. Additional experiments using RNA homopolymers found that polyG and polyI have procoagulant activity similar to polyphosphate, while polyA and polyC are not procoagulant. Thus, the procoagulant activity of RNA is rather highly dependent on base composition. PMID:29719836

  15. Addition of a sequence from α2-antiplasmin transforms human serum albumin into a blood clot component that speeds clot lysis

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    Gataiance Sharon

    2009-03-01

    Full Text Available Abstract Background The plasma protein α2-antiplasmin (α2AP is cross-linked to fibrin in blood clots by the transglutaminase factor XIIIa, and in that location retards clot lysis. Competition for this effect could be clinically useful in patients with thrombosis. We hypothesized that fusion of N-terminal portions of α2-antiplasmin to human serum albumin (HSA and production of the chimeric proteins in Pichia pastoris yeast would produce a stable and effective competitor protein. Results Fusion protein α2AP(13-42-HSA was efficiently secreted from transformed yeast and purified preparations contained within a mixed population the full-length intact form, while fusions with longer α2AP moieties were inefficiently secreted and/or degraded. The α2AP(13-42-HSA protein, but not recombinant HSA, was cross-linked to both chemical lysine donors and fibrin or fibrinogen by factor XIIIa, although with less rapid kinetics than native α2AP. Excess α2AP(13-42-HSA competed with α2AP for cross-linking to chemical lysine donors more effectively than a synthetic α2AP(13-42 peptide, and reduced the α2AP-dependent resistance to fibrinolysis of plasma clots equally effectively as the peptide. Native α2AP was found in in vivo clots in rabbits to a greater extent than α2AP(13-42, however. Conclusion In this first report of transfer of transglutamination substrate status from one plasma protein to another, fusion protein α2AP(13-42-HSA was shown to satisfy initial requirements for a long-lasting, well-tolerated competitive inhibitor of α2-antiplasmin predicted to act in a clot-localized manner.

  16. Clot formation and lysis in platelet rich plasma of healthy donors and patients with resistant hypertension

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    I. I. Patalakh

    2018-04-01

    Full Text Available Hemostatic balance in blood is affected by numerous factors, including coagulation and fibrinolytic proteins, the wide spectrum of their inhibitors, and blood cells. Since platelets can participate in contradictory processes, they significantly complicate the whole picture. Therefore, nowadays the development of global assays of hemostasis, which can reflect the physiological process of hemostasis and can be used for point-of-care diagnosis of thrombosis, is crucial. This paper outlines a new approach we used to analyze the capabilities of clot waveform analysis tools to distinguish the response of platelet-rich plasma from healthy donors and patients with arterial hypertension caused by stimulation of coagulation and lysis (with exogenous thrombin and recombinant tissue-type plasminogen activator, respectively. In donor plasma, when the clot degradation was accompanied by 40 IU/ml of recombinant tissue-type plasminogen activator, platelets potentiated fibrinolysis more than coagulation, which ultimately shifts the overall balance to a profibrinolytic state. At the same time, for patients with hypertension, platelets, embedded in clot obtained from platelet-rich plasma, showed a weaker ability to stimulate fibrinolysis. The obtained data gives the evidence that platelets can act not only as procoagulants but also as profibrinolytics. By simultaneously amplifying coagulation and fibrinolysis, making their rates comparable, platelets would control plasma procoagulant activity, thereby regulating local hemostatic balance, the size and lifetime of the clot. Moreover, clot waveform analysis may be used to distinguish the effects of platelet-rich plasma on clotting or lysis of fibrin clots in healthy donors and patients with essential hypertension.

  17. PEMANFAATAN MILK CLOTTING ENZYME DARI Lactobacillus casei D11 UNTUK PEMBUATAN KEJU MOZZARELLA [Utilization of Milk Clotting Enzyme from Lactobacillus casei D11 for Mozzarella Cheese Making

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    Rohmatussolihat -

    2015-07-01

    Full Text Available Milk Clotting Enzyme (MCE is an active agent for cheese making which may be produced by Lactic acid bacteria (LAB. MCE activity differs according to the LAB strains used. Lactobacillus casei D11 could produced MCE when it is grown in MRS broth medium. In this study, MCE of L. casei D11 with the addition of rennet is used and optimized for the production of mozzarella cheese using Response Surface Method (RSM with Central Composite Design (CCD. The organoleptic properties were determined by hedonics test involving 30 respondents and analyzed statistically which was followed by a Duncan's test. Furthermore, a proximate analysis of mozzarella cheese was conducted. Our results show that the MCE activity produced by L. casei D11 was 8.471 Soxhlet Unit with protease activity of 3.28 U/mL. The ANOVA results showed that the concentration of MCE significantly influence the production of curd. Theoptimum concentration of MCE and rennet for the production of curd suited for the production of mozzarella cheese were 20 and 0.002%, respectively, with a maximum predicted curd yield of 14.996% (g/100 mL milk which is increased by 13.9% as compared to the curd yield before optimization. The statistical analysis on taste, color, flavor, and cheese texture by respondents shows that mozzarella cheese made by a combination of 15% of MCE and 0.00079 and 0.0015% of rennet, were organoleptically superior to the commercial mozzarella used in this experiment. The proximate analysis shows that mozzarella produced has a moisture content of 33.34%(w/w, 3.48% ash, 30.44% fat, 25.12% protein, 7.53% carbohydrate and energy of 404 kkal/100g.

  18. Validity and reliability of the session-RPE method for quantifying training load in karate athletes.

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    Tabben, M; Tourny, C; Haddad, M; Chaabane, H; Chamari, K; Coquart, J B

    2015-04-24

    To test the construct validity and reliability of the session rating of perceived exertion (sRPE) method by examining the relationship between RPE and physiological parameters (heart rate: HR and blood lactate concentration: [La --] ) and the correlations between sRPE and two HR--based methods for quantifying internal training load (Banister's method and Edwards's method) during karate training camp. Eighteen elite karate athletes: ten men (age: 24.2 ± 2.3 y, body mass: 71.2 ± 9.0 kg, body fat: 8.2 ± 1.3% and height: 178 ± 7 cm) and eight women (age: 22.6 ± 1.2 y, body mass: 59.8 ± 8.4 kg, body fat: 20.2 ± 4.4%, height: 169 ± 4 cm) were included in the study. During training camp, subjects participated in eight karate--training sessions including three training modes (4 tactical--technical, 2 technical--development, and 2 randori training), during which RPE, HR, and [La -- ] were recorded. Significant correlations were found between RPE and physiological parameters (percentage of maximal HR: r = 0.75, 95% CI = 0.64--0.86; [La --] : r = 0.62, 95% CI = 0.49--0.75; P training load ( r = 0.65--0.95; P reliability of the same intensity across training sessions (Cronbach's α = 0.81, 95% CI = 0.61--0.92). This study demonstrates that the sRPE method is valid for quantifying internal training load and intensity in karate.

  19. Chemometric approach for development, optimization, and validation of different chromatographic methods for separation of opium alkaloids.

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    Acevska, J; Stefkov, G; Petkovska, R; Kulevanova, S; Dimitrovska, A

    2012-05-01

    The excessive and continuously growing interest in the simultaneous determination of poppy alkaloids imposes the development and optimization of convenient high-throughput methods for the assessment of the qualitative and quantitative profile of alkaloids in poppy straw. Systematic optimization of two chromatographic methods (gas chromatography (GC)/flame ionization detector (FID)/mass spectrometry (MS) and reversed-phase (RP)-high-performance liquid chromatography (HPLC)/diode array detector (DAD)) for the separation of alkaloids from Papaver somniferum L. (Papaveraceae) was carried out. The effects of various conditions on the predefined chromatographic descriptors were investigated using chemometrics. A full factorial linear design of experiments for determining the relationship between chromatographic conditions and the retention behavior of the analytes was used. Central composite circumscribed design was utilized for the final method optimization. By conducting the optimization of the methods in very rational manner, a great deal of excessive and unproductive laboratory research work was avoided. The developed chromatographic methods were validated and compared in line with the resolving power, sensitivity, accuracy, speed, cost, ecological aspects, and compatibility with the poppy straw extraction procedure. The separation of the opium alkaloids using the GC/FID/MS method was achieved within 10 min, avoiding any derivatization step. This method has a stronger resolving power, shorter analysis time, better cost/effectiveness factor than the RP-HPLC/DAD method and is in line with the "green trend" of the analysis. The RP-HPLC/DAD method on the other hand displayed better sensitivity for all tested alkaloids. The proposed methods provide both fast screening and an accurate content assessment of the six alkaloids in the poppy samples obtained from the selection program of Papaver strains.

  20. Development and comparison of a minimally-invasive model of autologous clot pulmonary embolism in Sprague-Dawley and Copenhagen rats

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    Sanapareddy Nina

    2010-02-01

    Full Text Available Abstract Background Experimental models of pulmonary embolism (PE that produce pulmonary hypertension (PH employ many different methods of inducing acute pulmonary occlusion. Many of these models induce PE with intravenous injection of exogenous impervious objects that may not completely reproduce the physiological properties of autologous thromboembolism. Current literature lacks a simple, well-described rat model of autlogous PE. Objective: Test if moderate-severity autologous PE in Sprague-Dawley (SD and Copenhagen (Cop rats can produce persistent PH. Methods blood was withdrawn from the jugular vein, treated with thrombin-Ca++ and re-injected following pretreatment with tranexamic acid. Hemodynamic values, clot weights and biochemical measurements were performed at 1 and 5 days. Results Infusion of clot significantly increased the right ventricular peak systolic pressure to 45-55 mm Hg, followed by normalization within 24 hours in SD rats, and within 5 days in COP rats. Clot lysis was 95% (24 hours and 97% (5 days in SD rats and was significantly lower in COP rats (70%, 24 hours; 87% 5 days. Plasma D-dimer was elevated in surgical sham animals and was further increased 8 hours after pulmonary embolism. Neither strain showed a significant increase in bronchoalveolar chemotactic activity, myeloperoxidase activity, leukocyte infiltration, or chemokine accumulation, indicating that there was no significant pulmonary inflammation. Conclusions Both SD and COP rats exhibited near complete fibrinolysis of autologous clot PE within 5 days. Neither strain developed persistent PH. Experimental models of PE designed to induce sustained PH and a robust inflammatory response appear to require significant, persistent pulmonary vascular occlusion.