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Validation of Rapid Enzymatic Quantification of Acetic Acid In
foods Article Validation of Rapid Enzymatic Quantification of Acetic Acid in Vinegar on Automated Spectrophotometric System Irene Dini 1,* , Ritamaria Di Lorenzo 1, Antonello Senatore 2, Daniele Coppola 2 and Sonia Laneri 1 1 Department of Pharmacy, University of Naples Federico II, Via Domenico Montesano 49, 80131 Napoli, Italy; [email protected] (R.D.L.); [email protected] (S.L.) 2 Lcm Laboratory for Product Analysis of Chamber of Commerce, Corso Meridionale, 80143 Napoli, Italy; [email protected] (A.S.); [email protected] (D.C.) * Correspondence: [email protected] Received: 9 May 2020; Accepted: 4 June 2020; Published: 9 June 2020 Abstract: Vinegar is produced from the fermentation of agricultural materials and diluted acetic acid (diluted with water to 4–30% by volume) via sequential ethanol and acetic acid fermentation. The concentration of acetic acid must be measured during vinegar production. A Community method for analyzing acetic acid in vinegar is a non-specific method based on the assumption that the total acid concentration of the vinegar is attributable to the acetic acid. It consists of titration with a strong base in the presence of an indicator. This test is laborious and has a time-consuming character. In this work, a highly specific automated enzymatic method was validated, for the first time, to quantify the acetic acid in the wine vinegar, in terms of linearity, precision, repeatability, and uncertainty measurement. The results were compared to the Community method of analysis. Regression coefficient 1 and the normal distribution of residuals in the ANOVA test confirmed the method’s linearity. -
Standardizing Analytical Methods
Chapter 5 Standardizing Analytical Methods Chapter Overview 5A Analytical Standards 5B Calibrating the Signal (Stotal) 5C Determining the Sensitivity (kA) 5D Linear Regression and Calibration Curves 5E Compensating for the Reagent Blank (Sreag) 5F Using Excel and R for a Regression Analysis 5G Key Terms 5H Chapter Summary 5I Problems 5J Solutions to Practice Exercises The American Chemical Society’s Committee on Environmental Improvement defines standardization as the process of determining the relationship between the signal and the amount of analyte in a sample.1 In Chapter 3 we defined this relationship as SktotalA=+nSA reagtor Skotal = AAC where Stotal is the signal, nA is the moles of analyte, CA is the analyte’s concentration, kA is the method’s sensitivity for the analyte, and Sreag is the contribution to Stotal from sources other than the sample. To standardize a method we must determine values for kA and Sreag. Strategies for accomplishing this are the subject of this chapter. 1 ACS Committee on Environmental Improvement “Guidelines for Data Acquisition and Data Quality Evaluation in Environmental Chemistry,” Anal. Chem. 1980, 52, 2242–2249. 147 148 Analytical Chemistry 2.1 5A Analytical Standards To standardize an analytical method we use standards that contain known amounts of analyte. The accuracy of a standardization, therefore, depends on the quality of the reagents and the glassware we use to prepare these standards. For example, in an acid–base titration the stoichiometry of the acid–base reaction defines the relationship between the moles of analyte and the moles of titrant. In turn, the moles of titrant is the product of the See Chapter 9 for a thorough discussion of titrant’s concentration and the volume of titrant used to reach the equiva- titrimetric methods of analysis. -
Calorimetry of 4-Aminopyridine Alan Everett Av N Til Iowa State University
Iowa State University Capstones, Theses and Retrospective Theses and Dissertations Dissertations 1976 Calorimetry of 4-aminopyridine Alan Everett aV n Til Iowa State University Follow this and additional works at: https://lib.dr.iastate.edu/rtd Part of the Analytical Chemistry Commons Recommended Citation Van Til, Alan Everett, "Calorimetry of 4-aminopyridine " (1976). Retrospective Theses and Dissertations. 6229. https://lib.dr.iastate.edu/rtd/6229 This Dissertation is brought to you for free and open access by the Iowa State University Capstones, Theses and Dissertations at Iowa State University Digital Repository. It has been accepted for inclusion in Retrospective Theses and Dissertations by an authorized administrator of Iowa State University Digital Repository. For more information, please contact [email protected]. INFORMATION TO USERS This material was produced from a microfilm copy of the original document. While the most advanced technological means to photograph and reproduce this document have been used, the quality is heavily dependent upon the quality of the original submitted. The following explanation of techniques is provided to help you understand markings or patterns which may appear on this reproduction. 1.The sign or "target" for pages apparently lacking from the document photographed is "Missing Page(s)". If it was possible to obtain the missing page(s) or section, they are spliced into the film along with adjacent pages. This may have necessitated cutting thru an image and duplicating adjacent pages to insure you complete continuity. 2. When an image on the film is obliterated with a large round black mark, it is an indication that the photographer suspected that the copy may have moved during exposure and thus cause a blurred image. -
Lecture 10. Analytical Chemistry
Lecture 10. Analytical Chemistry Basic concepts 1 What is Analytical Chemistry ? It deals with: • separation • identification • determination of components in a sample. It includes coverage of chemical equilibrium and statistical treatment of data. It encompasses any type of tests that provide information relating to the chemical composition of a sample. 2 • Analytical chemistry is divided into two areas of analysis: • Qualitative – recognizes the particles which are present in a sample. • Quantitative – identifies how much of particles is present in a sample. 3 • The substance to be analyzed within a sample is known as an analyte, whereas the substances which may cause incorrect or inaccurate results are known as chemical interferents. 4 Qualitative analysis 5 Qualitative analysis is used to separate an analyte from interferents existing in a sample and to detect the previous one. ➢It gives negative, positive, or yes/no types of data. ➢It informs whether or not the analyte is present in a sample. 6 Examples of qualitative analysis 7 8 9 Analysis of an inorganic sample The classical procedure for systematic analysis of an inorganic sample consists of several parts: ➢preliminary tests (heating, solubility in water, appearance of moisture) ➢ more complicated tests e.g. ✓introducing the sample into a flame and noting the colour produced; ➢determination of anionic or cationic constituents of solute dissolved in water 10 Flame test Solutions of ions, when mixed with concentrated HCl and heated on a nickel/chromium wire in a flame, cause the -
Atomic Absorption Spectroscopy
ATOMIC ABSORPTION SPECTROSCOPY Edited by Muhammad Akhyar Farrukh Atomic Absorption Spectroscopy Edited by Muhammad Akhyar Farrukh Published by InTech Janeza Trdine 9, 51000 Rijeka, Croatia Copyright © 2011 InTech All chapters are Open Access distributed under the Creative Commons Attribution 3.0 license, which allows users to download, copy and build upon published articles even for commercial purposes, as long as the author and publisher are properly credited, which ensures maximum dissemination and a wider impact of our publications. After this work has been published by InTech, authors have the right to republish it, in whole or part, in any publication of which they are the author, and to make other personal use of the work. Any republication, referencing or personal use of the work must explicitly identify the original source. As for readers, this license allows users to download, copy and build upon published chapters even for commercial purposes, as long as the author and publisher are properly credited, which ensures maximum dissemination and a wider impact of our publications. Notice Statements and opinions expressed in the chapters are these of the individual contributors and not necessarily those of the editors or publisher. No responsibility is accepted for the accuracy of information contained in the published chapters. The publisher assumes no responsibility for any damage or injury to persons or property arising out of the use of any materials, instructions, methods or ideas contained in the book. Publishing Process Manager Anja Filipovic Technical Editor Teodora Smiljanic Cover Designer InTech Design Team Image Copyright kjpargeter, 2011. DepositPhotos First published January, 2012 Printed in Croatia A free online edition of this book is available at www.intechopen.com Additional hard copies can be obtained from [email protected] Atomic Absorption Spectroscopy, Edited by Muhammad Akhyar Farrukh p. -
Quantitative NMR As a Versatile Tool for the Reference Material Preparation
magnetochemistry Review Quantitative NMR as a Versatile Tool for the Reference Material Preparation Kihwan Choi 1,* , Sangki Myoung 2, Yejin Seo 2 and Sangdoo Ahn 2,* 1 Organic Metrology Group, Division of Chemical and Biological Metrology, Korea Research Institute of Standards and Science, Daejeon 34113, Korea 2 Department of Chemistry, Chung-Ang University, Seoul 06974, Korea; [email protected] (S.M.); [email protected] (Y.S.) * Correspondence: [email protected] (K.C.); [email protected] (S.A.); Tel.: +82-42-868-5557 (K.C.); +82-2-820-5230 (S.A.) Abstract: The assessment of primary calibrator purity is critical for establishing traceability to the International System of Units (SI). Recently, quantitative nuclear magnetic resonance (qNMR) has been used as a purity determination method for reference material development, and many related measurement techniques have been designed to acquire accurate and reliable results. This review introduces the recent advances in these techniques (including multidimensional methods), focusing on the application of qNMR to reference material preparation. Keywords: qNMR; reference material; purity assay 1. Introduction The establishment of metrological traceability is important for achieving the compa- Citation: Choi, K.; Myoung, S.; Seo, Y.; rability of measurement results [1]. In regard to chemical measurements, traceability to Ahn, S. Quantitative NMR as a the International System of Units (SI) is realized through the use of calibration standards Versatile Tool for the Reference having certified purity values [2]. The purity of primary calibrators has been traditionally Material Preparation. determined by the mass balance method, that is, by subtracting the total amount of im- Magnetochemistry 2021, 7, 15. -
Viewed, Most SPME Extractions Are Performed in Aqueous Matrices.11,16 the Organic Solvent Most Likely Acted As an Interference with the Analyte Extraction
A COMPARISON OF COMMON LABORATORY TECHNIQUES FOR THE ANALYSIS OF THIOCARBAMATE PESTICIDES A Thesis Presented to The Graduate Faculty of The University of Akron In Partial Fulfillment of the Requirements for the Degree Master of Science Tammy Schumacher Donohue August, 2012 A COMPARISON OF COMMON LABORATORY TECHNIQUES FOR THE ANALYSIS OF THIOCARBAMATE PESTICIDES Tammy Schumacher Donohue Thesis Approved: Accepted: ________________________________ ________________________________ Advisor Dean of the College Dr. Claire Tessier Dr. Chand Midha ________________________________ ________________________________ Faculty Reader Dean of the Graduate School Dr. Kim C. Calvo Dr. George R. Newkome ________________________________ ________________________________ Department Chair Date Dr. Kim C. Calvo ii ABSTRACT The United States Environmental Protection Agency has devised a set of regulations limiting the use of thiocarbamate pesticides for the health and safety of humans and the environment. These regulations dictate the maximum amount of thiocarbamate compounds that may be released or present in soil, waste, and groundwater. Therefore, it is important to be able to determine their concentration accurately and reproducibly. A study was conducted to determine the best way to identify and quantify six thiocarbamate herbicides using equipment commonly found in industrial laboratories. Three analytical methods were tested: gas chromatography-mass spectrometry, high performance liquid chromatography, and infrared spectroscopy. They were chosen for their common usage, broad application, and operative ability. A comparison of these methods was made to determine the most effective technique for thiocarbamate identification and quantification. iii DEDICATION To my husband, Chris, whose steadfast belief in me never wavered. Thank you for always letting me know you were behind me, no matter what. I love you. -
Guidance for the Validation of Analytical Methodology and Calibration of Equipment Used for Testing of Illicit Drugs in Seized Materials and Biological Specimens
Vienna International Centre, PO Box 500, 1400 Vienna, Austria Tel.: (+43-1) 26060-0, Fax: (+43-1) 26060-5866, www.unodc.org Guidance for the Validation of Analytical Methodology and Calibration of Equipment used for Testing of Illicit Drugs in Seized Materials and Biological Specimens FOR UNITED NATIONS USE ONLY United Nations publication ISBN 978-92-1-148243-0 Sales No. E.09.XI.16 *0984578*Printed in Austria ST/NAR/41 V.09-84578—October 2009—200 A commitment to quality and continuous improvement Photo credits: UNODC Photo Library Laboratory and Scientific Section UNITED NATIONS OFFICE ON DRUGS AND CRIME Vienna Guidance for the Validation of Analytical Methodology and Calibration of Equipment used for Testing of Illicit Drugs in Seized Materials and Biological Specimens A commitment to quality and continuous improvement UNITED NATIONS New York, 2009 Acknowledgements This manual was produced by the Laboratory and Scientific Section (LSS) of the United Nations Office on Drugs and Crime (UNODC) and its preparation was coor- dinated by Iphigenia Naidis and Satu Turpeinen, staff of UNODC LSS (headed by Justice Tettey). LSS wishes to express its appreciation and thanks to the members of the Standing Panel of the UNODC’s International Quality Assurance Programme, Dr. Robert Anderson, Dr. Robert Bramley, Dr. David Clarke, and Dr. Pirjo Lillsunde, for the conceptualization of this manual, their valuable contributions, the review and finali- zation of the document.* *Contact details of named individuals can be requested from the UNODC Laboratory and Scientific Section (P.O. Box 500, 1400 Vienna, Austria). ST/NAR/41 UNITED NATIONS PUBLICATION Sales No. -
Limit of Detection for Calibration Methods
Limit of detection for calibration methods MARÍA JOSÉ RODRÍGUEZ CUESTA Doctoral Thesis ROVIRA I VIRGILI UNIVERSITY Tarragona 2006 UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 Limit of detection for second-order calibration methods Doctoral thesis ROVIRA I VIRGILI UNIVERSITY UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 Rovira i Virgili University Department of Analytical Chemistry and Organic Chemistry Limit of detection for second-order calibration methods Dissertation presented by María José Rodríguez Cuesta to receive the degree Doctor of the Rovira i Virgili University European PhD Tarragona, 2006 Supervisor Dr. Ricard Boqué i Martí UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 UNIVERSITAT ROVIRA I VIRGILI LIMIT OF DETECTION FOR SECOND-ORDER CALIBRATION METHODS. M. José Rodríguez Cuesta ISBN: 978-84-690-7787-0 / DL: T.1349-2007 ROVIRA I VIRGILI UNIVERSITY Department of Analytical Chemistry and Organic Chemistry Dr -
Bioanalytical Method Validation and Its Pharmaceutical Application
A tica nal eu yt c ic a a m A r a c t Sonawane et al., Pharm Anal Acta 2014, 5:3 h a P DOI: 10.4172/2153-2435.1000288 ISSN: 2153-2435 Pharmaceutica Analytica Acta Review Article Open Access Bioanalytical Method Validation and Its Pharmaceutical Application- A Review Lalit V Sonawane*, Bhagwat N Poul, Sharad V Usnale, Pradeepkumar V Waghmare and Laxman H Surwase Department of Quality Assurance, MSS’s Maharashtra College of Pharmacy, Nilanga, Maharashtra, India Abstract Bioanalytical methods, based on a variety of physico-chemical and biological techniques such as chromatography, immunoassay and mass spectrometry, must be validated prior to and during use to give confidence in the results generated. It is the process used to establish that a quantitative analytical method is suitable for biomedical applications. Bioanalytical method validation includes all of the procedures that demonstrate that a particular method used for quantitative measurement of analytes in a given biological matrix, such as blood, plasma, serum, or urine is reliable and reproducible for the intended use. The present manuscript focuses on the consistent evaluation of the key bioanalytical validation parameters is discussed: accuracy, precision, sensitivity, selectivity, standard curve, limits of quantification, range, recovery and stability. These validation parameters are described, together with an example of validation methodology applied in the case of chromatographic methods used in bioanalysis, taking in account to the recent Food and Drug Administration (FDA) guidelines and EMA guidelines. Keywords: Bioanalytical method validation; Validation parameters; Bioanalytical method validation is vital not only in terms of Application; FDA and EMA guidelines regulatory submission but also for ensuring generation of high quality data during drug discovery and development. -
Method 6800: Elemental and Molecular Speciated Isotope
METHOD 6800 ELEMENTAL AND MOLECULAR SPECIATED ISOTOPE DILUTION MASS SPECTROMETRY SW-846 is not intended to be an analytical training manual. Therefore, method procedures are written based on the assumption that they will be performed by analysts who are formally trained in at least the basic principles of chemical analysis and in the use of the subject technology. In addition, SW-846 methods, with the exception of required method use for the analysis of method-defined parameters, are intended to be guidance methods which contain general information on how to perform an analytical procedure or technique which a laboratory can use as a basic starting point for generating its own detailed standard operating procedure (SOP), either for its own general use or for a specific project application. The performance data included in this method are for guidance purposes only, and are not intended to be and must not be used as absolute quality control (QC) acceptance criteria for purposes of laboratory accreditation. 1.0 SCOPE AND APPLICATION For a summary of changes in this version from the previously published draft method 6800, February 2007 Rev 0, please see Appendix A at the end of this document. 1.1 This method consists of two approaches: (1) isotope dilution mass spectrometry (IDMS) for the determination of the total concentrations of elements and molecules and (2) molecular speciated isotope dilution mass spectrometry (SIDMS) for the determination of elemental and molecular species. IUPAC defines speciation analysis as “analyzing chemical compounds that differ in isotopic composition, conformation, oxidation or electronic state, or in the nature of their complexed or covalently bound substituents, which can be regarded as distinct chemical species.” This method is applicable to the determination of total elements as well as elemental species and molecular species at parts per billion (ppb), parts per trillion (ppt) and sub-ppt levels in samples of various types; in waters, solids, blood, foods or in extracts or digests. -
Univariate and Multivariate Analysis of Phosphorus Element in Fertilizers Using Laser-Induced Breakdown Spectroscopy
sensors Article Univariate and Multivariate Analysis of Phosphorus Element in Fertilizers Using Laser-Induced Breakdown Spectroscopy Baohua Zhang 1,*, Pengpeng Ling 2, Wen Sha 2, Yongcheng Jiang 2 and Zhifeng Cui 3 1 School of Electronics and Information Engineering, Anhui University, Hefei 230061, China 2 School of Electric Engineering and Automation, Anhui University, Hefei 230601, China; [email protected] (P.L.); [email protected] (W.S.); [email protected] (Y.J.) 3 Institute of Atomic and Molecular Physics, Anhui Normal University, Wuhu 241000, China; [email protected] * Correspondence: [email protected]; Tel.: +86-551-6386-1237 Received: 5 March 2019; Accepted: 9 April 2019; Published: 11 April 2019 Abstract: Rapid detection of phosphorus (P) element is beneficial to the control of compound fertilizer production process and is of great significance in the fertilizer industry. The aim of this work was to compare the univariate and multivariate analysis of phosphorus element in compound fertilizers and obtain a reliable and accurate method for rapid detection of phosphorus element. A total of 47 fertilizer samples were collected from the production line; 36 samples were used as a calibration set, and 11 samples were used as a prediction set. The univariate calibration curve was constructed by the intensity of characteristic line and the concentration of P. The linear correlation coefficient was 0.854 as the existence of the matrix effect. In order to eliminate the matrix effect, the internal standardization as the appropriate methodology was used to increase the accuracy. Using silicon (Si) element as an internal element, a linear correlation coefficient of 0.932 was obtained.