Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235nm / 280 nm UV Absorbance Ratio
|
|
- Abigayle Anna Brooks
- 8 years ago
- Views:
Transcription
1 an ABC Laboratories white paper Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235nm / 280 nm UV Absorbance Ratio A. Sen, R. Dunphy, L. Rosik Analytical Bio-Chemistry Laboratories
2 Copyright Notice Copyright Analytical Bio-Chemistry Laboratories, Inc All Rights Reserved. Unless otherwise indicated, all materials on these pages are copyrighted by ABC Laboratories. No part of this publication may be reproduced for commercial use without ABC Laboratories express consent. Copying tables, figures, or excerpts with proper attribution is permitted for noncommercial use, on the condition that proper attribution of the source in all copies is provided; however, this does not grant permission to publish. In referencing this work, please observe the following preferred citation: A.Sen, R. Dunphy, and L. Rosik. Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldahyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio. ABC Laboratories, Analytical Bio-Chemistry Laboratories, Inc. i Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
3 Table of Contents Abstract... Introduction... Experimental... Results and Discussion... Conclusions... References ii Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
4 Abstract The 235 nm/280 nm UV absorbance ratio (UV Ratio) is widely used as a measure of the degree of polymerization of glutaraldehyde. Conventional practice is to measure the UV absorbance of bulk material at 235 nm (C=C absorption) and at 280 nm (C=O absorption). Gel permeation chromatography of preparations of heat-treated glutaraldehyde (HTGA) did not have sufficient mass discrimination to explain the variation in the UV Ratio of HTGA. Preparations of HTGA were analyzed by direct infusion ion trap mass spectrometry (IT-MS) and time of flight mass spectrometry (TOF-MS). Structures were assigned to the masses found. The structures of the UV-absorbing species were used to calculate absorbance contributions from each species found in the preparations at greater than 5% relative abundance. The contributions were weighted and summed. A MS-based UV Ratio was calculated and compared to the experimentally determined UV Ratio for the HTGA preparations. A very good correlation was obtained. 1 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
5 Introduction Polymerized glutaraldehyde has been used as a fixative agent for electron microscopy and to immobilize proteins for decades (1-5). The solution chemistry of glutaraldehyde has been reviewed (2). The UV Ratio is a parameter that has been used classically to describe the extent of polymerization of the material (3,4,7,8). An additional analytical method was developed to better characterize the polymeric mixture and correlate to this absorbance ratio. Development data from a low molecular weight SEC method resulted in nearly the same molecular weight values for all four of the HTGA samples examined (Mp = 377 to 384 Da) which had UV Ratios of from 2 to 20. This suggested that the UV Ratio (degree of polymerization) was not simply molecular weight dependent but was also dependent on the structures of the oligomers present. The existing literature seems to support this (1,3,6-9). Direct infusion mass spectra of the HTGA preparations were acquired. A simple weighted average molecular weight was calculated for the samples (based on the masses seen and their relative abundances in each sample) and was found to not correlate to the UV Ratio, as was seen for the SEC results. From the MS data the structures were assigned for the various types of oligomers present. Based on these structures and the published values for the mass extinction coefficients of the chromophores (1) in the oligomers a MSbased UV Ratio was calculated for the bulk HTGA. 2 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
6 Experimental The HTGA samples were prepared in water and heat treated. The samples had varying degrees of polymerization as indicated by their UV Ratio, as shown in Table 1. The HTGA samples were diluted 1:1 with a 0.1% formic acid aqueous solution for mass spectrometric analysis. Table 1: HTGA Samples The diluted samples were analyzed on a Thermo Fleet Ion Trap Mass Spectrometer by direct infusion into the electrospray ionization (ESI) source using the onboard syringe pump at a flow rate ~ 15 µl/ min. Data was collected for the range of m/z 50 to 1000 for two minutes and the data from the entire infusion was averaged. Earlier SEC work with these samples had indicated that the vast majority of the sample would be below 1000 Da. The MS thus obtained for 74, 78-2, 78-1, and 78-3 are shown in Figure 1, Figure 2, Figure 3, and Figure 4 respectively. The majority of the structures could be assigned from this data. Note that due to the sodium content of the samples the ions seen are sodiated cations that are +23 u from the actual neutral masses of the oligomers of interest. Some peaks seen were not readily assigned based on these spectra. The samples were also analyzed by Waters Micromass LCT Premier Time of Flight Mass Spectrometer in order to obtain empirical formulae for the ions of interest and thus allow complete structural assignments. Direct infusion into the electrospray ionization (ESI) source using a syringe pump at a flow rate ~ 15 µl/min. Data was collected for the range of m/z 50 to 1000 for two minutes and the data from the entire infusion was averaged. 3 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
7 Experimental (cont) Figure 1: Mass Spectrum of Sample 74 Figure 2: Mass Spectrum of Sample Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
8 Experimental (cont) Figure 3: Mass Spectrum of Sample 78-1 Figure 4: Mass Spectrum of Sample Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
9 Results and Discussion The acetal family of oligomers were the most predominant series of compounds seen in the aqueous samples. Their general structure is shown in Figure 5 along with the mass assignments and two example structures. These oligomers have no chromophores and so do not contribute to the UV Ratio. This is why the UV Ratio does not correlate to the average molecular weight of the sample. These compounds therefore were not included in the calculation. Figure 5: The Acetal Family of Oligomers The aldol condensation family of oligomers were also seen in the samples. Their general structure is shown in Figure 6 along with the mass assignments and two example structures. Figure 6: The Aldol Condensation Family of Oligomers 6 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
10 Results and Discussion (cont) The aldol condensation family of oligomers shown above in Figure 6 can also undergo the elimination of water to give compounds with some of the aldol linkages dehydrated to yield unsaturated aldehydes. Their general structure is shown in Figure 7 and Table 2, along with the mass assignments and two example structures. Figure 7: The Partially Dehydrated Aldol Condensation Family of Oligomers Table 2 The aldol condensation oligomers shown in Figure 6 have suffered aerobic oxidation to the diacids. Their general structure is shown in Figure 8 along with the mass assignments and two example structures. 7 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
11 Results and Discussion (cont) The aldol condensation family of oligomers shown above in Figure 6 can also undergo the elimination of water to give compounds with some of the aldol linkages dehydrated to yield unsaturated aldehydes. Their general structure is shown in Figure 7 and Table 2, along with the mass assignments and two example structures. Figure 8: The Oxidized Aldol Condensation Family of Oligomers The above assignments are in agreement with previous UV, IR, and NMR studies (1,2,6,9). There were no significant peaks found in the sample spectra that corresponded to oxidized and partially dehydrated oligomers. This was also the case for mono-oxidized and partially dehydrated species. Calculation of the MS-Based 235 nm/280 nm UV Absorbance Ratio The structural assignments are in agreement with previous UV, IR, and NMR studies (1,2,6,9). Once the structures for all of the significant peaks have been assigned then the UV absorbance contributions for each molecule can be calculated. The aldehydes moieties absorb at 280 nm and the carbon-carbon double bond absorbs at 235 nm. The mass extinction coefficients for the unconjugated aldehyde group, the conjugated aldehyde group, and the conjugated carbon-carbon double bond have been given as 0.042, 0.41, and 18.6 L/g cm (1). Therefore, for each relevant mass (structure that has a UV absorbance) the number of each kind of contributing chromophore can be determined by inspection. Those contributions to the 280 nm or the 235 nm absorptions can then be summed. These summed contributions can then be weighted with the relative abundance of the peak in the MS to give weighted 280 nm and 235 nm absorptions. The weighted absorptions can then be summed9 for all the relevant molecules in a sample and the UV Ratio calculated. The MS-based UV Ratio can then be correlated to the experimentally determined UV Ratio by regression. Summaries of this calculation for the samples 3.5% HTGA, 15% HTGA-1, 15% HTGA-2, and 15% HTGA-3 are shown in Figure 9, Figure 10, Figure 11, and Figure 12 respectively. A co-efficient of determination (R 2 ) value of was obtained and is show in Figure Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
12 Results and Discussion (cont) Figure 9: MS-Based UV Ratio of Sample 74 Figure 10: MS-Based UV Ratio of Sample Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
13 Results and Discussion (cont) Figure 11: MS-Based UV Ratio of Sample 78-1 Figure 12: MS-Based UV Ratio of Sample Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
14 Results and Discussion (cont) Figure 13: Correlation of Experimental UV Ratio to the MS-Based UV Ratio 11 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
15 Conclusions Preparations of HTGA were analyzed by direct infusion MS and structures were assigned to the masses found. The structures of the UV-absorbing species were used to calculate absorbance contributions from each species found in the preparations at greater than 5% relative abundance. The contributions were weighted and summed and a MS-based UV Ratio was calculated and compared to the experimentally determined UV Ratio for the HTGA preparations. Very good correlation was obtained. 12 Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
16 References 1. Margel S. and Rembaum A., Macromolecules 1980, 13, Mignealt I. et al., BioTechniques 2004, 37, Prento P., Histochemical Journal 1995, 27, Jones G.J., Journal of Histochemistry and Cytochemistry 1974, 22, Goff C.W. and Oster M.O., Journal of Histochemistry and Cytochemistry 1974, 22, Aso C. and Aito Y., Die Makromolekulare Chemie 1962, 58, Anderson P.J., Journal of Histochemistry and Cytochemistry 1967, 15, Frigerio N.A. and Shaw M.J., Journal of Histochemistry and Cytochemistry 1969, 17, Hardy P.M. et al., Chemical Communications 1969, Correlation of the Mass Spectrometric Analysis of Heat-Treated Glutaraldehyde Preparations to Their 235 nm/280 nm UV Absorbance Ratio
17 Analytical Bio-Chemistry (ABC) Laboratories, Inc Discovery Drive Columbia, Missouri Phone: Fax: Web: Analytical Bio-Chemistry Laboratories, Inc.
PosterREPRINT AN LC/MS ORTHOGONAL TOF (TIME OF FLIGHT) MASS SPECTROMETER WITH INCREASED TRANSMISSION, RESOLUTION, AND DYNAMIC RANGE OVERVIEW
OVERVIEW Exact mass LC/MS analysis using an orthogonal acceleration time of flight (oa-tof) mass spectrometer is a well-established technique with a broad range of applications. These include elemental
More informationPesticide Analysis by Mass Spectrometry
Pesticide Analysis by Mass Spectrometry Purpose: The purpose of this assignment is to introduce concepts of mass spectrometry (MS) as they pertain to the qualitative and quantitative analysis of organochlorine
More informationUltraviolet Spectroscopy
Ultraviolet Spectroscopy The wavelength of UV and visible light are substantially shorter than the wavelength of infrared radiation. The UV spectrum ranges from 100 to 400 nm. A UV-Vis spectrophotometer
More information13C NMR Spectroscopy
13 C NMR Spectroscopy Introduction Nuclear magnetic resonance spectroscopy (NMR) is the most powerful tool available for structural determination. A nucleus with an odd number of protons, an odd number
More informationAMD Analysis & Technology AG
AMD Analysis & Technology AG Application Note 120419 Author: Karl-Heinz Maurer APCI-MS Trace Analysis of volatile organic compounds in ambient air A) Introduction Trace analysis of volatile organic compounds
More informationElectrospray Ion Trap Mass Spectrometry. Introduction
Electrospray Ion Source Electrospray Ion Trap Mass Spectrometry Introduction The key to using MS for solutions is the ability to transfer your analytes into the vacuum of the mass spectrometer as ionic
More informationSimultaneous Metabolite Identification and Quantitation with UV Data Integration Using LightSight Software Version 2.2
Technical ote Simultaneous Metabolite Identification and Quantitation with UV Data Integration Using LightSight Software Version 2.2 Alek. Dooley, Carmai Seto, esham Ghobarah, and Elliott B. Jones verview:
More informationInfrared Spectroscopy 紅 外 線 光 譜 儀
Infrared Spectroscopy 紅 外 線 光 譜 儀 Introduction Spectroscopy is an analytical technique which helps determine structure. It destroys little or no sample (nondestructive method). The amount of light absorbed
More informationF321 THE STRUCTURE OF ATOMS. ATOMS Atoms consist of a number of fundamental particles, the most important are... in the nucleus of an atom
Atomic Structure F32 TE STRUCTURE OF ATOMS ATOMS Atoms consist of a number of fundamental particles, the most important are... Mass / kg Charge / C Relative mass Relative Charge PROTON NEUTRON ELECTRON
More information[ Care and Use Manual ]
PREP Calibration Mix DIOS Low i. Introduction Pre-packaged PREP Calibration Mixtures eliminate the need to purchase and store large quantities of the component calibration reagents, simplifying sample
More informationApplication of a New Immobilization H/D Exchange Protocol: A Calmodulin Study
Application of a New Immobilization H/D Exchange Protocol: A Calmodulin Study Jiang Zhao; Mei Zhu; Daryl E. Gilblin; Michael L. Gross Washington University Center for Biomrdical and Bioorganic Mass Spectrometry:
More information0 10 20 30 40 50 60 70 m/z
Mass spectrum for the ionization of acetone MS of Acetone + Relative Abundance CH 3 H 3 C O + M 15 (loss of methyl) + O H 3 C CH 3 43 58 0 10 20 30 40 50 60 70 m/z It is difficult to identify the ions
More informationfor mass spectrometry calibration tools Thermo Scientific Pierce Controls and Standards for Mass Spectrometry
Thermo Scientific Pierce Controls and Standards for Mass Spectrometry calibration tools for mass spectrometry Ensure confidence in instrument performance with Thermo Scientific Pierce Calibration Solutions
More informationOverview. Purpose. Methods. Results
A ovel Approach to Quantify Unbound Cisplatin, Carboplatin, and xaliplatin in Human Plasma Ultrafiltrate by Measuring Platinum-DDTC Complex Using LC/M/M Min Meng, Ryan Kuntz, Al Fontanet, and Patrick K.
More informationOrganic Spectroscopy. UV - Ultraviolet-Visible Spectroscopy. !! 200-800 nm. Methods for structure determination of organic compounds:
Organic Spectroscopy Methods for structure determination of organic compounds: X-ray rystallography rystall structures Mass spectroscopy Molecular formula -----------------------------------------------------------------------------
More informationMass Spectrometry. Overview
Mass Spectrometry Overview Mass Spectrometry is an analytic technique that utilizes the degree of deflection of charged particles by a magnetic field to find the relative masses of molecular ions and fragments.2
More informationOverview. Triple quadrupole (MS/MS) systems provide in comparison to single quadrupole (MS) systems: Introduction
Advantages of Using Triple Quadrupole over Single Quadrupole Mass Spectrometry to Quantify and Identify the Presence of Pesticides in Water and Soil Samples André Schreiber AB SCIEX Concord, Ontario (Canada)
More informationOrganic Spectroscopy
1 Organic Spectroscopy Second Year, Michaelmas term, 8 lectures: Dr TDW Claridge & Prof BG Davis Lectures 1 4 highlight the importance of spectroscopic methods in the structural elucidation of organic
More informationIntroduction to Proteomics 1.0
Introduction to Proteomics 1.0 CMSP Workshop Tim Griffin Associate Professor, BMBB Faculty Director, CMSP Objectives Why are we here? For participants: Learn basics of MS-based proteomics Learn what s
More informationL. Yu et al. Correspondence to: Q. Zhang (dkwzhang@ucdavis.edu)
Supplement of Atmos. Chem. Phys. Discuss., 5, 967 974, 5 http://www.atmos-chem-phys-discuss.net/5/967/5/ doi:.594/acpd-5-967-5-supplement Author(s) 5. CC Attribution. License. Supplement of Molecular transformations
More informationHenry Shion, Robert Birdsall, Steve Cubbedge, and Weibin Chen Waters Corporation, Milford, MA, USA APPLICATION BENEFITS INTRODUCTION WATERS SOLUTIONS
Development of Integrated Informatics Workflows for the Automated Assessment of Comparability for Antibody Drug Conjugates (ADCs) Using LC-UV and LC-UV/MS Henry Shion, Robert Birdsall, Steve Cubbedge,
More informationMicromass LCT User s Guide
Micromass LCT User s Guide 1) Log on to MassLynx with your username & password. 2) After you have logged in, the MassLynx software will automatically run. 3) After MassLynx has come up, open your project
More informationDaniel M. Mueller, Katharina M. Rentsch Institut für Klinische Chemie, Universitätsspital Zürich, CH-8091 Zürich, Schweiz
Toxichem Krimtech 211;78(Special Issue):324 Online extraction LC-MS n method for the detection of drugs in urine, serum and heparinized plasma Daniel M. Mueller, Katharina M. Rentsch Institut für Klinische
More informationAccurate calibration of on-line Time of Flight Mass Spectrometer (TOF-MS) for high molecular weight combustion product analysis
Accurate calibration of on-line Time of Flight Mass Spectrometer (TOF-MS) for high molecular weight combustion product analysis B. Apicella*, M. Passaro**, X. Wang***, N. Spinelli**** mariadellarcopassaro@gmail.com
More informationINFRARED SPECTROSCOPY (IR)
INFRARED SPECTROSCOPY (IR) Theory and Interpretation of IR spectra ASSIGNED READINGS Introduction to technique 25 (p. 833-834 in lab textbook) Uses of the Infrared Spectrum (p. 847-853) Look over pages
More informationelectron does not become part of the compound; one electron goes in but two electrons come out.
Characterization Techniques for Organic Compounds. When we run a reaction in the laboratory or when we isolate a compound from nature, one of our first tasks is to identify the compound that we have obtained.
More informationApplication Note # LCMS-62 Walk-Up Ion Trap Mass Spectrometer System in a Multi-User Environment Using Compass OpenAccess Software
Application Note # LCMS-62 Walk-Up Ion Trap Mass Spectrometer System in a Multi-User Environment Using Compass OpenAccess Software Abstract Presented here is a case study of a walk-up liquid chromatography
More informationCalculating Nucleic Acid or Protein Concentration Using the GloMax Multi+ Microplate Instrument
Calculating Nucleic Acid or Protein Concentration Using the GloMax Multi+ Microplate Instrument Technical Note INTRODUCTION Direct measurements of nucleic acid samples at OD 260 or protein samples at OD
More informationSymmetric Stretch: allows molecule to move through space
BACKGROUND INFORMATION Infrared Spectroscopy Before introducing the subject of IR spectroscopy, we must first review some aspects of the electromagnetic spectrum. The electromagnetic spectrum is composed
More informationFor example: (Example is from page 50 of the Thinkbook)
SOLVING COMBINED SPECTROSCOPY PROBLEMS: Lecture Supplement: page 50-53 in Thinkbook CFQ s and PP s: page 216 241 in Thinkbook Introduction: The structure of an unknown molecule can be determined using
More informationUHPLC/MS: An Efficient Tool for Determination of Illicit Drugs
Application Note: 439 UHPLC/MS: An Efficient Tool for Determination of Illicit Drugs Guifeng Jiang, Thermo Fisher Scientific, San Jose, CA, USA Key Words Accela UHPLC System MSQ Plus MS Detector Drugs
More informationHOMEWORK PROBLEMS: IR SPECTROSCOPY AND 13C NMR. The peak at 1720 indicates a C=O bond (carbonyl). One possibility is acetone:
HMEWRK PRBLEMS: IR SPECTRSCPY AND 13C NMR 1. You find a bottle on the shelf only labeled C 3 H 6. You take an IR spectrum of the compound and find major peaks at 2950, 1720, and 1400 cm -1. Draw a molecule
More informationDRUG METABOLISM. Drug discovery & development solutions FOR DRUG METABOLISM
DRUG METABLISM Drug discovery & development solutions FR DRUG METABLISM Fast and efficient metabolite identification is critical in today s drug discovery pipeline. The goal is to achieve rapid structural
More informationAmount of Substance. http://www.avogadro.co.uk/definitions/elemcompmix.htm
Page 1 of 14 Amount of Substance Key terms in this chapter are: Element Compound Mixture Atom Molecule Ion Relative Atomic Mass Avogadro constant Mole Isotope Relative Isotopic Mass Relative Molecular
More informationGetting the most from this book...4 About this book...5
Contents Getting the most from this book...4 About this book....5 Content Guidance Topic 1 Atomic structure and the periodic table...8 Topic 2 Bonding and structure...14 Topic 2A Bonding....14 Topic 2B
More informationTips & Tricks GPC/SEC: Analysis and Calibration For Low Molar Mass Macromolecules
GPC/SEC: Analysis and Calibration For Low Molar Mass Macromolecules Daniela Held, Silvia Fugmann, and Peter Kilz, PSS Polymer Standards Service GmbH, Mainz, Germany. Macromolecules can range from several
More informationLC-MS/MS for Chromatographers
LC-MS/MS for Chromatographers An introduction to the use of LC-MS/MS, with an emphasis on the analysis of drugs in biological matrices LC-MS/MS for Chromatographers An introduction to the use of LC-MS/MS,
More informationSuggested solutions for Chapter 3
s for Chapter PRBLEM Assuming that the molecular ion is the base peak (00% abundance) what peaks would appear in the mass spectrum of each of these molecules: (a) C5Br (b) C60 (c) C64Br In cases (a) and
More informationHigh Resolution LC-MS Data Output and Analysis
High Resolution LC-MS Data Output and Analysis Your Sample LC/MS Result Sample Sample Efficient Separation Preparation Introduction Gradient (column) Today Data (computer) LC- MS Ions Detection Ions Separation
More information2.02 DETERMINATION OF THE FORMULA OF A COMPLEX BY SPECTROPHOTOMETRY
2nd/3rd Year Physical Chemistry Practical Course, Oxford University 2.02 DETERMINATION OF THE FORMULA OF A COMPLEX BY SPECTROPHOTOMETRY (4 points) Outline Spectrometry is widely used to monitor the progress
More informationGuide to Reverse Phase SpinColumns Chromatography for Sample Prep
Guide to Reverse Phase SpinColumns Chromatography for Sample Prep www.harvardapparatus.com Contents Introduction...2-3 Modes of Separation...4-6 Spin Column Efficiency...7-8 Fast Protein Analysis...9 Specifications...10
More informationSpectrophotometry and the Beer-Lambert Law: An Important Analytical Technique in Chemistry
Spectrophotometry and the Beer-Lambert Law: An Important Analytical Technique in Chemistry Jon H. Hardesty, PhD and Bassam Attili, PhD Collin College Department of Chemistry Introduction: In the last lab
More informationOverview. Introduction. AB SCIEX MPX -2 High Throughput TripleTOF 4600 LC/MS/MS System
Investigating the use of the AB SCIEX TripleTOF 4600 LC/MS/MS System for High Throughput Screening of Synthetic Cannabinoids/Metabolites in Human Urine AB SCIEX MPX -2 High Throughput TripleTOF 4600 LC/MS/MS
More informationAnalyzing Small Molecules by EI and GC-MS. July 2014
Analyzing Small Molecules by EI and GC-MS July 2014 Samples Appropriate for GC-MS Volatile and semi-volatile organic compounds Rule of thumb,
More informationChem101: General Chemistry Lecture 9 Acids and Bases
: General Chemistry Lecture 9 Acids and Bases I. Introduction A. In chemistry, and particularly biochemistry, water is the most common solvent 1. In studying acids and bases we are going to see that water
More informationSex Hormone Testing by Mass Spectrometry
Sex Hormone Testing by Mass Spectrometry Robert L. Fitzgerald, PhD, DABCC Professor of Pathology University of California-San Diego San Diego, CA, 92161 rfitzgerald@ucsd.edu Learning Objectives After this
More informationLC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research
LC-MS/MS Method for the Determination of Docetaxel in Human Serum for Clinical Research J. Jones, J. Denbigh, Thermo Fisher Scientific, Runcorn, Cheshire, UK Application Note 20581 Key Words SPE, SOLA,
More informationUV-Visible Spectroscopy
UV-Visible Spectroscopy UV-Visible Spectroscopy What is UV-Visible Spectroscopy? Molecular spectroscopy that involves study of the interaction of Ultra violet (UV)-Visible radiation with molecules What
More informationAnalysis of Free Bromate Ions in Tap Water using an ACQUITY UPLC BEH Amide Column
Analysis of Free Bromate Ions in Tap Water using an ACQUITY UPLC BEH Amide Column Sachiki Shimizu, FUJIFILM Fine Chemicals Co., Ltd., Kanagawa, Japan Kenneth J. Fountain, Kevin Jenkins, and Yoko Tsuda,
More informationNMR and other Instrumental Techniques in Chemistry and the proposed National Curriculum.
NMR and other Instrumental Techniques in Chemistry and the proposed National Curriculum. Dr. John Jackowski Chair of Science, Head of Chemistry Scotch College Melbourne john.jackowski@scotch.vic.edu.au
More informationChapter 5 Classification of Organic Compounds by Solubility
Chapter 5 Classification of Organic Compounds by Solubility Deductions based upon interpretation of simple solubility tests can be extremely useful in organic structure determination. Both solubility and
More informationIdentification of Unknown Organic Compounds
Identification of Unknown Organic Compounds Introduction The identification and characterization of the structures of unknown substances are an important part of organic chemistry. Although it is often
More informationSimultaneous qualitative and quantitative analysis using the Agilent 6540 Accurate-Mass Q-TOF
Simultaneous qualitative and quantitative analysis using the Agilent 654 Accurate-Mass Q-TOF Technical Overview Authors Pat Perkins Anabel Fandino Lester Taylor Agilent Technologies, Inc. Santa Clara,
More informationMonoclonal Antibody Fragment Separation and Characterization Using Size Exclusion Chromatography Coupled with Mass Spectrometry
Monoclonal ntibody Fragment Separation and haracterization Using Size Exclusion hromatography oupled with Mass Spectrometry uthors Haiying hen Katherine McLaughlin Sepax Technologies, Inc. 5 Innovation
More informationIntroduction to mass spectrometry (MS) based proteomics and metabolomics
Introduction to mass spectrometry (MS) based proteomics and metabolomics Tianwei Yu Department of Biostatistics and Bioinformatics Rollins School of Public Health Emory University September 10, 2015 Background
More informationChapter 1: Moles and equations. Learning outcomes. you should be able to:
Chapter 1: Moles and equations 1 Learning outcomes you should be able to: define and use the terms: relative atomic mass, isotopic mass and formula mass based on the 12 C scale perform calculations, including
More informationChemical Structure of the polymer showing end groups: CH 3 CH 2 CH H
Polymer Reference Materials-Polystyrene Introduction Reference materials are used for calibration and performance evaluation of instruments used as part of overall quality assurance programs of polymer.
More informationResearch for leachables of nuclear grade cation exchange resin
International Journal of Smart Grid and Clean Energy Research for leachables of nuclear grade cation exchange resin Liang-Cheng Chen, Dah-Yu Kao, Tung-Jen Wen, Ping-Ji Huang Institute of Nuclear Energy
More informationApplication of Structure-Based LC/MS Database Management for Forensic Analysis
Cozette M. Cuppett and Michael P. Balogh Waters Corporation, Milford, MA USA Antony Williams, Vitaly Lashin and Ilya Troisky Advanced Chemistry Development, Toronto, ntario, Canada verview Application
More informationThe Unshifted Atom-A Simpler Method of Deriving Vibrational Modes of Molecular Symmetries
Est. 1984 ORIENTAL JOURNAL OF CHEMISTRY An International Open Free Access, Peer Reviewed Research Journal www.orientjchem.org ISSN: 0970-020 X CODEN: OJCHEG 2012, Vol. 28, No. (1): Pg. 189-202 The Unshifted
More informationIB Chemistry. DP Chemistry Review
DP Chemistry Review Topic 1: Quantitative chemistry 1.1 The mole concept and Avogadro s constant Assessment statement Apply the mole concept to substances. Determine the number of particles and the amount
More informationE35 SPECTROSCOPIC TECHNIQUES IN ORGANIC CHEMISTRY
E35 SPECTRSCPIC TECNIQUES IN RGANIC CEMISTRY TE TASK To use mass spectrometry and IR, UV/vis and NMR spectroscopy to identify organic compounds. TE SKILLS By the end of the experiment you should be able
More informationOrganic Chemistry Tenth Edition
Organic Chemistry Tenth Edition T. W. Graham Solomons Craig B. Fryhle Welcome to CHM 22 Organic Chemisty II Chapters 2 (IR), 9, 3-20. Chapter 2 and Chapter 9 Spectroscopy (interaction of molecule with
More informationChapter 13 Spectroscopy NMR, IR, MS, UV-Vis
Chapter 13 Spectroscopy NMR, IR, MS, UV-Vis Main points of the chapter 1. Hydrogen Nuclear Magnetic Resonance a. Splitting or coupling (what s next to what) b. Chemical shifts (what type is it) c. Integration
More informationMULTIPLE CHOICE. Choose the one alternative that best completes the statement or answers the question.
Exam Name 1) Which compound would be expected to show intense IR absorption at 3300 cm-1? A) butane B) CH3CH2C CH C)CH3C CCH3 D) but-1-ene 1) 2) Which compound would be expected to show intense IR absorption
More informationProton Nuclear Magnetic Resonance Spectroscopy
Proton Nuclear Magnetic Resonance Spectroscopy Introduction: The NMR Spectrum serves as a great resource in determining the structure of an organic compound by revealing the hydrogen and carbon skeleton.
More informationChemistry 4631. Instrumental Analysis Lecture 1. Chem 4631
Chemistry 4631 Instrumental Analysis Lecture 1 Syllabus Chemistry 4631 Spring 2016 Lecture: MWF 9:00 9:50 a.m. Chem 352 Attendance is expected. Instructor: Dr. Teresa D. Golden Chem 279, 565-2888, tgolden@unt.edu.
More informationSTANFORD UNIVERSITY MASS SPECTROMETRY 333 CAMPUS DR., MUDD 175 STANFORD, CA 94305-5080
Training on the ZQ Open access MS Questions? Contact Dr. Allis Chien allis@stanford.edu 650-723-0710 0710 STANFORD UNIVERSITY MASS SPECTROMETRY STANFORD UNIVERSITY MASS SPECTROMETRY 333 CAMPUS DR., MUDD
More informationDiscovery of Pesticide Protomers Using Routine Ion Mobility Screening
Michael McCullagh, 1 David Eatough, 1 Vincent Hanot, 2 and Séverine Goscinny 2 1 Waters Corporation, Wilmslow, UK 2 Wetenschappelijk Instituut Volksgezondheid Institut Scientifique de Santé Publique, Brussels,
More informationDetermination of Molecular Structure by MOLECULAR SPECTROSCOPY
Determination of Molecular Structure by MOLEULAR SPETROSOPY hemistry 3 B.Z. Shakhashiri Fall 29 Much of what we know about molecular structure has been learned by observing and analyzing how electromagnetic
More informationA Ratiometric NMR ph Sensing Strategy Based on Slow- Proton-Exchange (SPE) Mechanism
Electronic Supplementary Material (ESI) for Chemical Science. This journal is The Royal Society of Chemistry 2015 A Ratiometric NMR ph Sensing Strategy Based on Slow- Proton-Exchange (SPE) Mechanism Loïse
More informationCalculation of Molar Masses. Molar Mass. Solutions. Solutions
Molar Mass Molar mass = Mass in grams of one mole of any element, numerically equal to its atomic weight Molar mass of molecules can be determined from the chemical formula and molar masses of elements
More informationCoordination Compounds with Copper (II) Prelab (Week 2)
Coordination Compounds with Copper (II) Prelab (Week 2) Name Total /10 SHOW ALL WORK NO WORK = NO CREDIT 1. What is the purpose of this experiment? 2. Write the generic chemical formula for the coordination
More informationIUCLID 5 COMPOSITION AND ANALYSIS GUIDANCE DOCUMENT: IRON ORES, AGGLOMERATES [EINECS NUMBER 265 996 3, CAS NUMBER 65996 65 8] IRON ORE PELLETS
IUCLID 5 COMPOSITION AND ANALYSIS GUIDANCE DOCUMENT: IRON ORES, AGGLOMERATES [EINECS NUMBER 265 996 3, CAS NUMBER 65996 65 8] IRON ORE PELLETS INTRODUCTION Each REACH registrant is required to file its
More informationAssessment Schedule 2013 Chemistry: Demonstrate understanding of the properties of organic compounds (91391)
NCEA Level 3 Chemistry (91391) 2013 page 1 of 8 Assessment Schedule 2013 Chemistry: Demonstrate understanding of the properties of organic compounds (91391) Evidence Statement Q Evidence Achievement Achievement
More informationPage 1. 6. Which hydrocarbon is a member of the alkane series? (1) 1. Which is the structural formula of methane? (1) (2) (2) (3) (3) (4) (4)
1. Which is the structural formula of methane? 6. Which hydrocarbon is a member of the alkane series? 7. How many carbon atoms are contained in an ethyl group? 1 3 2 4 2. In the alkane series, each molecule
More informationCHEM 51LB EXP 1 SPECTROSCOPIC METHODS: INFRARED AND NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
CHEM 51LB EXP 1 SPECTRSCPIC METHDS: INFRARED AND NUCLEAR MAGNETIC RESNANCE SPECTRSCPY REACTINS: None TECHNIQUES: IR Spectroscopy, NMR Spectroscopy Infrared (IR) and nuclear magnetic resonance (NMR) spectroscopy
More informationTechnical Report. Automatic Identification and Semi-quantitative Analysis of Psychotropic Drugs in Serum Using GC/MS Forensic Toxicological Database
C146-E175A Technical Report Automatic Identification and Semi-quantitative Analysis of Psychotropic Drugs in Serum Using GC/MS Forensic Toxicological Database Hitoshi Tsuchihashi 1 Abstract: A sample consisting
More informationAnalysis of the Vitamin B Complex in Infant Formula Samples by LC-MS/MS
Analysis of the Vitamin B Complex in Infant Formula Samples by LC-MS/MS Stephen Lock 1 and Matthew Noestheden 2 1 AB SCIEX Warrington, Cheshire (UK), 2 AB SCIEX Concord, Ontario (Canada) Overview A rapid,
More informationNuclear Structure. particle relative charge relative mass proton +1 1 atomic mass unit neutron 0 1 atomic mass unit electron -1 negligible mass
Protons, neutrons and electrons Nuclear Structure particle relative charge relative mass proton 1 1 atomic mass unit neutron 0 1 atomic mass unit electron -1 negligible mass Protons and neutrons make up
More informationCHEMICAL FORMULAS AND FORMULA WEIGHT CALCULATIONS
CHEMICAL FORMULAS AND FORMULA WEIGHT CALCULATIONS 1. THE MEANING OF A CHEMICAL FORMULA A chemical formula is a shorthand method of representing the elements in a compound. The formula shows the formulas
More informationAtomic Masses. Chapter 3. Stoichiometry. Chemical Stoichiometry. Mass and Moles of a Substance. Average Atomic Mass
Atomic Masses Chapter 3 Stoichiometry 1 atomic mass unit (amu) = 1/12 of the mass of a 12 C atom so one 12 C atom has a mass of 12 amu (exact number). From mass spectrometry: 13 C/ 12 C = 1.0836129 amu
More information2015 2016 Ph.D. Science & Engineering Positions. Wilmington, DE. Analytical Sciences Wilmington, DE. Sciences Wilmington, DE.
2015 2016 Ph.D. Science & Engineering Positions 1) Synthetic Organic Chemistry Crop Protection Newark, DE 2) Polymer Chemistry Performance Polymers Various 3) Polymer Engineering Performance Polymers Various
More informationAppendix 5 Overview of requirements in English
Appendix 5 Overview of requirements in English This document is a translation of Appendix 4 (Bilag 4) section 2. This translation is meant as a service for the bidder and in case of any differences between
More informationNUVISAN Pharma Services
NUVISAN Pharma Services CESI MS Now available! 1st CRO in Europe! At the highest levels of quality. LABORATORY SERVICES Equipment update STATE OF THE ART AT NUVISAN CESI MS Now available! 1st CRO in Europe!
More informationMethod Development of LC-MS/MS Analysis of Aminoglycoside Drugs: Challenges and Solutions
Method Development of LC-MS/MS Analysis of Aminoglycoside Drugs: Challenges and Solutions authors Angela (Qi) Shen, Ling Morgan, Marcele L. Barroso, and Xin Zhang; Tandem Labs Tuyen Nguyen; Sepracor Inc.
More informationUV-Vis Vis spectroscopy. Electronic absorption spectroscopy
UV-Vis Vis spectroscopy Electronic absorption spectroscopy Absortpion spectroscopy Provide information about presence and absence of unsaturated functional groups Useful adjunct to IR Determination of
More informationSUCRALOSE. White to off-white, practically odourless crystalline powder
SUCRALOSE Prepared at the 41st JECFA (1993), published in FNP 52 Add 2 (1993). Metals and arsenic specifications revised at the 63rd JECFA (2004). An ADI of 0-15 mg/kg bw was established at the 37th JECFA
More informationAuthenticity Assessment of Fruit Juices using LC-MS/MS and Metabolomic Data Processing
Authenticity Assessment of Fruit Juices using LC-MS/MS and Metabolomic Data Processing Lukas Vaclavik 1, Ondrej Lacina 1, André Schreiber 2, and Jana Hajslova 1 1 Institute of Chemical Technology, Prague
More informationAccurate Mass Screening Workflows for the Analysis of Novel Psychoactive Substances
Accurate Mass Screening Workflows for the Analysis of Novel Psychoactive Substances TripleTOF 5600 + LC/MS/MS System with MasterView Software Adrian M. Taylor AB Sciex Concord, Ontario (Canada) Overview
More information13.4 UV/VIS Spectroscopy
13.4 UV/VIS Spectroscopy The spectroscopy which utilizes the ultraviolet (UV) and visible (VIS) range of electromagnetic radiation, is frequently referred to as Electronic Spectroscopy. The term implies
More informationChemistry B11 Chapter 4 Chemical reactions
Chemistry B11 Chapter 4 Chemical reactions Chemical reactions are classified into five groups: A + B AB Synthesis reactions (Combination) H + O H O AB A + B Decomposition reactions (Analysis) NaCl Na +Cl
More informationLab 2 Biochemistry. Learning Objectives. Introduction. Lipid Structure and Role in Food. The lab has the following learning objectives.
1 Lab 2 Biochemistry Learning Objectives The lab has the following learning objectives. Investigate the role of double bonding in fatty acids, through models. Developing a calibration curve for a Benedict
More informationDefinition of the Measurand: CRP
A Reference Measurement System for C-reactive Protein David M. Bunk, Ph.D. Chemical Science and Technology Laboratory National Institute of Standards and Technology Definition of the Measurand: Human C-reactive
More information15/05/2008 Chemistry 231 Experiment 11 Lee 1 Cyclohexene from Cyclohexanol Larry Lee Partner: Ichiro Suzuki
15/05/2008 Chemistry 231 Experiment 11 Lee 1 Cyclohexene from Cyclohexanol Larry Lee Partner: Ichiro Suzuki bjective: The purpose of this experiment is to isolate Cyclohexene from Cyclohexanol by sulphuric
More informationChemistry. CHEMISTRY SYLLABUS, ASSESSMENT and UNIT PLANNERS GENERAL AIMS. Students should be able to
i CHEMISTRY SYLLABUS, ASSESSMENT and UNIT PLANNERS GENERAL AIMS Students should be able to - apply and use knowledge and methods that are typical to chemistry - develop experimental and investigative skills,
More information3. What would you predict for the intensity and binding energy for the 3p orbital for that of sulfur?
PSI AP Chemistry Periodic Trends MC Review Name Periodic Law and the Quantum Model Use the PES spectrum of Phosphorus below to answer questions 1-3. 1. Which peak corresponds to the 1s orbital? (A) 1.06
More informationDevelop a Quantitative Analytical Method for low (» 1 ppm) levels of Sulfate
Cantaurus, Vol. 7, 5-8, May 1999 McPherson College Division of Science and Technology Develop a Quantitative Analytical Method for low (» 1 ppm) levels of Sulfate Janet Bowen ABSTRACT Sulfate is used in
More informationNucleic Acid Purity Assessment using A 260 /A 280 Ratios
Nucleic Acid Purity Assessment using A 260 /A 280 Ratios A common practice in molecular biology is to perform a quick assessment of the purity of nucleic acid samples by determining the ratio of spectrophotometric
More information