Mass spectrometry analysis of oligonucleotide syntheses. If other spectroscopic data is available analyze fully confirm inferences from table 1 and presence of elements in table 2 step 5. Interpretation of mass spectra, 4th edition, by fred mclafferty, published by university science books, 0935702253. Interpretation of mass spectral data 1 the molecular ion. Interpreting protein mass spectra is a handson laboratory guide for a wide range of researchers investigating the structures of proteins and peptides. Chapter 2 fragmentation and interpretation of spectra 2. Mass spectrometry allows us to measure the masses of atoms and molecules, and also obtain information about their chemical structure. Feb 01, 2016 for the love of physics walter lewin may 16, 2011 duration.
It has contributed to numerous discoveries in chemistry, physics and biochemistry. A few types of mass spectrometers, for example some timeofflight instruments, have a higher resolution of r 5,000 to 50,000 or, ultimately, there are fticr mass spectrometers with a resolution of up to r 1,000,000. This simplified list will help you to interpret many spectra, however there are other mechanisms of fragmentation which cannot be covered in this brief tutorial. Esiqtof and malditof mass spectra of pei with h and oh end groups at the initiating x and terminating y chain end were shown in figure 1. Analysis of mass spectrometry data for protein identi cation in complex biological mixtures by. Nowadays standard libraries could include a few hundred thousands spectra.
Pdf on jun 7, 2017, teodor octavian nicolescu and others published interpretation of mass spectra find, read and cite all the research you need on. Lee, a beginners guide to mass spectral interpretation, 1998. It will be your resort to maintain downloading guide interpretation of mass spectra. If good inferences could be made, use the remainder of the mass spectrum to try. Mass spectrometry ms is a mainstream chemical analysis technique in the twentyfirst century. Well, with molecular ions or fragment ions that contain chlorine atoms, peaks can be seen at two different mass values owing to the significant abundance of the two isotopes. Swap data function is now available in the batch processing panel. A simple mass spectrum is represented by a two dimensional bar plot, the height of. Updated link to human metabolom database from mass to formula tool.
Interpretation of mass spectra, say the authors, aims at correlating ion dissociation mechanisms on a much broader scale, with emphasis on basic attributes such as ionization energies, proton affinities, and bond dissociation energies. Mass spectra can be quite complicated and interpretation difficult. The mass spectra of compounds a and b are nearly identical, except for the additional peak at 208. It may be necessary to report an extra significant digit, e.
How does an analyst know that a match has occurred when comparing mass spectra. Isotopic percentage and nominal mass calculation are also. If you are working with electron ionization ei or just staring to interpret your own spectra for low molecular weight species, this is your book. The focus is on the interpretation of structural information gathered through electrospray ionization mass spectrometry. Mass spectra of the 35 nonanes have been measured by the mass spectrometry section of this bureau as part of the program of measuring mass spcctra of pure hydrocarbons. Mass spectral interpretation is the method employed to identify the chemical formula, characteristic fragment patterns and possible fragment ions from the mass spectra. Interpreting mass spectra gcms data analysis gcms combines the advantages of both techniques the high resolving power and the speed of analysis of gc with the qualitative and. Imaging mass spectrometry can be used to reveal spatial distributions of multiple molecular species in a 2d biological sample. Database searching using uninterpreted msms spectra 31. This helps researcher to establish the branching pattern and verifying the basic unit of glycan.
Using the molecular ion to find the relative formula mass. Introduction mass spectrometry mass spec or ms uses high energy electrons to break a molecule into fragmentation. New algorithms and software tools for confident proteoform identification and quantification are needed. The mass spectra of simple hydrocarbons have peaks at mz values corresponding to the ions produced by breaking cc bonds. Driven by the need to identify, characterize, and quantify proteins at ever increasing sensitivity and in ever more complex samples, a wide range of new mass spectrometry. The masses of peaks 1, 2, 3, and 4 are successively smaller in mass by one. The fundamental concepts of ionization, fragmentation, and rearrangement of ions as found in mass spectra are covered in some detail, along with the.
Provides comprehensive coverage of the interpretation of lcmsms mass spectra of 0 drugs and pesticides. Interpretation of mass spectra in searchworks catalog. Volatile organic compounds by gas chromatography mass spectrometry gcms pdf pdf. Due to the large amount of data produced by this technology, it is. If you are trying to understand ms for high molecular weight proteins and such, i would recommend looking at introduction to mass spectrometry by j.
Lecture 3 mass spectrometry principles of mass spectrometry mass spectrometry separates molecules based on the mass to charge ratio. Mass spectrometry is a powerful technique that has been used to identify bacteria by their protein content and to assess bacterial functional traits through analysis of their specialized. May 07, 2015 chlorine can have atoms with a mass of 35, or a mass of 37. Pdf on jun 7, 2017, teodor octavian nicolescu and others published interpretation of mass spectra find, read and cite all the research you need on researchgate. Ham, even electron mass spectrometry with biomolecule. Students should be familiar with the operation of mass spectrometers and the presentation of mass spectra. Interpreting topdown mass spectra using spectral alignment. Examine spectrum for peak clusters of characteristic isotopic patterns.
For the analytical chemist, a mass spectrum is useful for two applications. Mass spectrometry and interpreting mass spectra compound. However, topdown mass spectra are substantially more complex than conventional bottomup data. Analysis of antibody drug conjugates adcs by native mass spectrometry on the bioaccord system henry shion, ying qing yu, and weibin chen waters corporation, milford, ma, usa figure 1. By convention, m is the numerical value for the mass. First, the fundamental notions of mass spectrometry are explained, so that the reader can easily cover this chapter graphs, main pick, molecular ion, illogical pick, nitrogen rule, etc. Explain why, and in doing so assign the labeled peaks in the mass spectrum. The exact mass of this elemental combination is, taking the mass of 12c as 12.
The tallest peak in the mass spectrum is called the base peak. Before we can calculate the mass of the compound we must determine the charge state of the two peaks. The most intense ion is assigned an abundance of 100, and it is referred to as thebase peak. Gas chromatographymass spectrometry gc ms interpretation of ei spectra jeremy keirsey ccic msp. A mass spectrum plural spectra is a plot of the ion signal as a function of the mass tocharge ratio. The fundamental di culty in the analysis of mass spectrometry. In the mass spectrum, the heaviest ion the one with the greatest mz value is likely to be the molecular ion. The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be analysed. Lecture notes in eimass spectrometry by torben lund. Mass spectrometry ms interpretation general interpretation strategies. Everyone who analyzes mass spectra already has an answer to this question, however, different analysts may use different criteria for evaluating the same data.
Best practice guide for generating mass spectra december 2006 vicki barwick, lgc john langley, university of southampton tony mallet, university of greenwich bridget stein, epsrc national mass spectrometry service centre ken webb, consultant isbn. Completely revised from the first edition, an updated and unified approach to mass spectral interpretation. At high energies, the ionising electron beam can fragment the molecule by cleaving particular bonds. Additional analysis if no inferences are realistic from tables 3 and 4, attempt deeper analysis of the mass spectrum. This is usually given an arbitrary height of 100, and the height of everything else is measured relative to this. The mass spectra are used to determine 1 the elemental signature, 2 the isotopic signature of a sample, 3 the mass of each individual particle, 4 the molecular mass and of the constituent molecules if the sample is a mixture, and 5 elucidation of the chemical structure of the molecule or molecules, if the sample is a mixture.
Common fragmentation processes for organic molecules are the mclafferty rearrangement and alpha cleavage. This transfer continues until the chemical potential of each substance in all. Mass spectrometry is a powerful technique in analytical chemistry that was. A basic approach, second edition combines coverage of the principles underlying mass spectral analysis with clear guidelines on how to apply them in a laboratory setting. Purchase interpretation of mass spectra of organic compounds 1st edition. Analysis of mass spectrometry data for protein identi. The nature of mass spectra a mass spectrum will usually be presented as a vertical bar graph, in which each bar represents an ion having a specific mass tocharge ratio mz and the length of the bar indicates the relative abundance of the ion. Mar 27, 2015 mass spectrometry mass spectrometry is the most accurate method for determining the molecular mass of the compound and its elemental composition. The mass to charge ratio mz is used to describe ions observed in mass spectrometry.
You may need a pdf reader to view some of the files on this page. Step 1 understand that the peak value observed in the spectrum equals mass divided by charge and that the mass is the mass of the molecule plus any adducts protons 190. This peak if it appears will be the highest mass peak in the spectrum. Sooner you get guide interpretation of mass spectra, by fred w. The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be. Interpretation of mass spectra of organic compounds 1st edition. Predict the structure of the molecules given by the following spectral data.
A mass spectrum can represent many different types of information based on the type of mass spectrometer and the specific experiment applied. The peak with the largest mz, however, will be due to the complete molecule and will be equal to the m r of the molecule. It will be your resort to maintain downloading guide interpretation of mass spectra, by fred w. Practical class exercises will apply fundamental principles used to interpret mass spectra. Data system mass detector analyzer vacuum system source inlet region more precisely mass spectrometry determines the mass of a molecule. Pdf interpretation of msms mass spectra of drugs and.
Pdf multivariate analysis of imaging mass spectrometry data. The fundamental concepts of ionization, fragmentation, and rearrangement of ions as found in mass spectra. The mass spectrum allows an experienced analyst to identify the compound or at a minimum narrow the possibilities down to a few compounds from the millions of. The results are typically presented as a mass spectrum, a plot of intensity as a function of the mass tocharge ratio. The leading scientist in this field was fred mclafferty who together with frantisek turecek has written a very famous text book. Esi and maldi tandem mass spectrometry of polyethylene. Interpreting esi spectra the y axis is labeled relative intensity.
Also, the students carry out a mass spectrometry experiment and learn to interpret the resulting mass spectra. Examples of fragmentation and the interpretation of mass spectra. Introduction mass spectrometry ms is an analytical technique that measures the mass tocharge particles. If good inferences could be made, use the remainder of the mass spectrum to try to elucidate structural features or isomerism. Interpretation of mass spectra of organic compounds.
A few compounds have mass spectra which dont contain a molecular ion peak, because all the molecular ions break into fragments. With contributions from noted experts from europe and north america, mass spectrometry instrumentation, interpretation, and applications serves as a forum to introduce students to the whole world of mass spectrometry. For methane the base peak is also the m peak molecular ion, although this is usually not the case. Using accurate mass measurement, this can be readily distinguished from the mass of butane c 4h 10 which is. Simglycan helps in interpreting a mass spectra by highlighting the experimental mz values that match those of theoretical fragments and generates an annotated spectrum depicting the loss of consecutive monosaccharide units. Mass spectrometry mass spectrometry is the most accurate method for determining the molecular mass of the compound and its elemental composition. The mass spectra are used to determine 1 the elemental signature, 2 the isotopic signature of a sample, 3 the mass of each individual particle, 4 the molecular mass and of the constituent. Mass spectrometry is a central analytical technique for protein research and for the study of biomolecules in general. This is caused by a different ion than the corresponding peak in the pentane mass spectrum. It is commonly used for the identification of organic compounds from electron ionization mass spectrometry.
Jan 01, 2003 comparisons can be made based on a variety of criteria. Introduction the united states and most of the world are exceedingly dependent on. The tallest line in the stick diagram in this case at mz 43 is called the base peak. Bibliography includes bibliographical references p. Interpretation of mass spectra of organic compounds outlines the basic instrumentation, sample handling techniques, and procedures used in the interpretation of mass spectra of organic compounds. In spme, the extraction occurs by the mass transfer of analytes from the sample to a polymer coating over a fusedsilica fiber.
Note that with dications, ions will normally be doubly charged, with mz half of the ion mass. The outcome has been widespread use of complex instrumentation, often as a walk up service, by staff with little education or training relevant to the task. Pdf download interpretation of mass spectra, by fred w. It is also called as positive ion spectra or line spectra. All but one of the spectra have been published in detail in the api catalog of mass spectral data 1. In the stick diagram showing the mass spectrum of pentane, the line produced by the heaviest ion passing through the machine at mz 72 is due to the molecular ion. Updated link to chemspider from mass to formula panel. The molecular fragmentation peaks in the mass spectrum can give clues as to the substructure of the molecule. Mass spectra is a plot of relative abundance against mass tocharge ratio. Interpretation of msms mass spectra of drugs and pesticides wilfried m. By convention, m is the numerical value for the mass of the ion and z is the numerical value for the charge of the ion.
Mass spectrometry ms is an analytical technique that measures the mass tocharge ratio of ions. Mass spectra and ir mass spectrometry measuring the m r of an organic molecule if a molecule is put through a mass spectrometer it will often break up and give a series of peaks caused by the fragments. Appearance of the mass spectrum formation of the mass spectrum mass analysis of ions ion abundance measurement sample introduction systems mixture analysis molecular structure information standard interpretation procedure general references 2 elemental composition. You might wish to refer to the table of bond dissociation energies when attempting problems involving the interpretation of mass spectra. Esi lcms spectrum of locusta migratoria cuticular protein 16512.