Mass spectral interpretation pdf

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. Most processes are very rapid, occurring within a few nano or microseconds. 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. Other atoms that have even molecular weights like carbon, oxygen, and. So far, weve looked at how chemists can determine the presence of particular bonds present in molecules with infrared spectroscopy, and how they can gain information about the structure of molecules using hydrogen and carbon nuclear magnetic resonance. The results are typically presented as a mass spectrum, a plot of intensity as a function of the mass tocharge ratio. Present fundamental concepts regarding mass spectral interpretation objectives at the end of this section you should be able to. Isotopes hold a special place not only in ms but also, in general terms, in chemistry and physics.

For larger molecules, it is common to see higher charge states, such as z 2 or z 3. A few compounds have mass spectra which dont contain a molecular ion peak, because all the molecular ions break into fragments. Mass defect from nuclear physics to mass spectral analysis. These strategies are what i noticed when i was completing the practice problems. Comprehensive structural characterization of phenolics in. Terrence lees book title, a beginners guide to mass spectral interpretation is quite accurate. Mass spectrometry of fatty acids a beginners guide part 1. Learn simple and easytounderstand lcms approaches for structure identification of metabolites, impurities, natural products, and biomolecules. Lecture notes in eimass spectrometry by torben lund.

Doesnt the multiple charging effect just serve to confound the interpretation. For singlycharged species z 1, the observed mass corresponds to the monoisotopic mass. It is a fundamental property of the nucleus and the principle behind nuclear energy. The survey scans were acquired in the orbitrap mass analyzer operating at 120,000 fwhm resolving power. Stein, technical leader william wallace, group leader evaluation. Ei spectra are rich in fragments thus useful in structure determination thro interpretation. Mass spectral interpretation pacs course number 10 registration form register by making a copy of this form and send it complete with contact and payment infomration to the address below.

Hundreds of research laboratories scattered all over the world use ms every day to investigate fundamental phenomena on. It has contributed to numerous discoveries in chemistry, physics and biochemistry. Sooner you get guide interpretation of mass spectra, by fred w. Please list your special interest on the registration form below. Jul 21, 2017 mass defect is associated with the binding energy of the nucleus. Mar 27, 2015 general steps in mass spectral interpretation 10. Nists webbook which includes ir, uvvis and mass spectra of many organic compounds. My thanks are extended to the staff of my facility n.

It is only an introduction and interested readers are encouraged to consult more specialized books and journal articles for additional details. List and explain the main characteristics of the mass spectrum explain how mass spectrometric data can be used for structure analysis explain why is important to optimise esiapci parameters. Sauerwein to use a large set of electron ionization mass spectra from the nistepanih mass spectral library is also gratefully acknowledged. Pdf a beginners guide to mass spectral interpretation. Dec 19, 2012 shows you how to get the information out of a mass spectrum and use it to help suggest the identity of an unidentified molecule. A mass range of 1002000 mz and a normalized collision energy of 30 was used for the survey scans. Protein sequencing and identification with mass spectrometry. Request pdf mass spectral interpretation the identification of metabolites is an integral part of the drug discovery and development process. Take your mass spec knowledge and skills to the next level with mass s selfpaced courses.

Mass defect has also entered into the mass spectrometry terminology with the availability of high resolution mass spectrometry and has found application in mass spectral analysis. The ionized molecule often fragments into smaller ionsradicals. The book emphasizes the use of this important analytical technique in many different. 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. Oct 05, 2007 he is the author of mass spectrometry desk reference. It is an excellent source of information for the mass spec novice. Interpreting electrospray mass spectra an ionsource. Version see revision notice the nist mass spectrometry data center stephen e. Mass spectroscopy mass spectroscopy is a technique causing the formation of the gaseous ions with or without fragmentation. Gross leads through the design of all types of mass analyzers and ionization methods to mass spectral interpretation and coupling techniques. Please create your bookmark, if you are interested in learning about mass spectrometry, mass spectral interpretation, instrumentation, and the full range of ionization methods. Approaches that analyze deglycosylated peptides using proteomics approaches are not included. Typical mass spectrometry research focuses on the formation of gas phase ions, the chemistry of ions, and applications of mass spectrometry. In mass spectrometry ms, the obvious concern is the actual masses of the atoms, molecules, or fragment thereof.

Mass spectrometry mass spectrometry is the most accurate method for determining the molecular mass of the compound and its elemental composition. Using the molecular ion to find the relative formula mass. The number of compounds with gc methodsri library in the ei ms library mainlib is 72,361. Mass spectrometry is a wideranging analytical technique, which involves the production. The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be analysed. 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 and to the many different perspectives that each scientific field brings to its use.

If good inferences could be made, use the remainder of the mass spectrum to try to elucidate structural features or isomerism. Nistepanih mass spectral library nist 05 and search. H 2, he, ne, ch 4, h 2 o, f, c 2 h 6, co, c 2 h 5oh, o 2, ar, c 3 h 8, co 2, kr however, in the common practise, the gas species of the residual gas are mixed and cannot be separated easily and quickly. While this is less useful in a more advanced spectroscopy. Mass spectrometry is used in many different fields and is applied to pure samples as well as complex mixtures. The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be.

The first mass spectral measurements were undertaken by j. In heterolytic cleavage, an electron pair moves together to the charged atom. With the multiple charging phenomena displayed in electrospray spectra how does one calculate the mass of a compound. A beginners guide to mass spectral interpretation terrence. As youve seen, the mass spectrum of even very similar organic compounds will be quite different because of the different fragmentation patterns that can occur.

Written by this well known professor and expert on mass spectral interpretation, it was purchased for use at work where we use ms every day. Gas chromatographymass spectrometry gc ms interpretation of ei spectra jeremy keirsey ccic msp. The expanding role of mass spectrometry in biotechnology 2nd edition. High mass accuracy is referred to as exact mass measurement, and when measuring the mass of a particular compound at the ppm level in mass accuracy, it is possible to unambiguously determine elemental composition. This paper covers the basics of mass spectrometry instrumentation and introduces the interpretation of mass spectra. Ms interpretation general interpretation strategies. Computerization of mass spectral data is also discussed. Aims and scope of mass spectrometry a textbook mass spectrometry today is an indispensable tool in chemistry and life sciences. Nominal mw will be an odd number if the compound also contains an odd. This website offers problems and solutions corresponding to each chapter of mass spectrometry a textbook, 3rd edition. Nitrogen has an even atomic mass but bonds with three other atoms in its most stable form. Mass spectral interpretation is the method employed to identify the chemical formula, characteristic fragment patterns and possible fragment ions from the mass spectra. He has developed and taught 10 sessions of an interactive web course on mass spectral interpretation over the past 4 years. The number of hits may also be reduced by taking an accurately measured isotope pattern of the ion into consideration.

Mass spectrometry and interpreting mass spectra compound. It is also called as positive ion spectra or line spectra. This peak if it appears will be the highest mass peak in the spectrum, except for isotope peaks. Mass spectrometry, analytical chemistry by open learning, wiley, 2nd edition 1999. 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. Allows specific compound identification structural elucidation via spectral interpretation. Gcms combines the advantages of both techniques the high resolving power and the speed of analysis of gc with the qualitative and quantitative analytical capabilities of the ms down to the ppb level.

Nistepanih mass spectral library nist 17 and nist mass spectral search program version 2. Software tools that calculate glycopeptide composition from msonly data will not be summarized in detail. If other spectroscopic data is available analyze fully confirm inferences from table 1 and presence of elements in table 2. A beginners guide to mass spectral interpretation 19 feb 2014. Interpretation of a mass spectrum is often compared to doing a jigsaw puzzle. Mass spectrometry ms is a mainstream chemical analysis technique in the twentyfirst century.

In mass spectrometry, one generates ions from a sample to be analyzed. Isotopic percentage and nominal mass calculation are also. Do not think of this as an algorithm but as second nature. The following is a summary of software tools for interpretation of intact glycopeptide mass spectral data. The mass to charge ratio mz is used to describe ions observed in mass spectrometry.

This book consists of nine chapters and begins with a historical overview of mass spectrometry. Using ms techniques to measure the ratio of 12 c to 14 c, one can determine the age of objects that incorporated 14 c into their structure such as once living fossils. This information is used to elucidate the chemical structures of molecules, such as pesticides or peptides. Nistepanih mass spectral library nist 17 and nist mass. Flock for their efforts and to the staff of the local libraries for their friendly support. It will be your resort to maintain downloading guide interpretation of mass spectra, by fred w. This rule is a result of nitrogens unique property. The 2017 version of the nistepanih mass spectral library nist 17 contains four mass spectral libraries and a library of retention index rigc method. Mass spectral interpretation using the rule of author. The guide arose from discussions held at the vam mass spectrometry. A read is counted each time someone views a publication summary such as the title, abstract, and list of authors, clicks on a figure, or views or downloads the fulltext.

Microsoft word guide to interpretation of mass spectra. From spectra, the mass of the molecular ion and fragments are used to determine the elemental composition or isotopic signature of a compound. Anzor mikaia, principal vladimir zaikin ei damo zhu ei. This page looks at how fragmentation patterns are formed when organic molecules are fed into a mass spectrometer, and how you can get information from the mass spectrum. Shows you how to get the information out of a mass spectrum and use it to help suggest the identity of an unidentified molecule. Lcms fundamentals and applications mass spectral intrepretation peptide and protein characterization optimization and validation of lcms methods.

Please bookmark this site, if you are interested in learning about mass spectrometry, mass spectral interpretation, instrumentation, and the full range of ionization methods such as ei, ci, fd, fab, maldi, and esi. For the analytical chemist, a mass spectrum is useful for two applications. The leading scientist in this field was fred mclafferty who together with frantisek turecek has written a very famous text book. Starting from the very principles of gasphase ion chemistry, isotopic composition, and accurate mass, jurgen h. Mass spectral determination of fasting tear glucose concentrations in nondiabetic volunteers, justin t. The fundamental concepts of ionization, fragmentation, and rearrangement of ions as found in mass spectra are covered in some detail, along with the rectangular array and interpretation maps. Interpretation of mass spectra of organic compounds. Comparative analysis of mass spectral matching for confident. Mclafferty sooner you get guide interpretation of mass spectra, by fred w. Mass spectra is a plot of relative abundance against mass tocharge ratio. Parent ion may be absent aliphatic alcohols, nitrites, nitrates, nitro.

Mass spectrometry works by ionizing chemical compounds to generate. For the fourth in the analytical chemistry series, we turn to mass spectrometry. Introduction to mass spectrometry wiley online books. The separation of pnp isomers was not optimized with one set of gc conditions. Mass spectral fragments of common hydrocarbons mass spectral peaks can be identified to have originated from the fragmentation of specific hydrocarbon sources including. Examine spectrum for peak clusters of characteristic isotopic patterns. When students ask what books to read on mass spectrometry, there are various excellent monographs, but the ideal textbook still seemed to be missing at least in my opinion. Rar a beginners guide to mass spectral interpretation pdf. Provided you have a computer data base of mass spectra, any unknown spectrum can be computer analyzed and simply matched against the data base. It is well written and he also stresses pitfalls students routinely make in analysis. Mass spectrometry a textbook, problems and solutions website. Chapter 2 fragmentation and interpretation of spectra 2. With higher resolution instruments, faster computers, larger and better spectral libraries, and more reliable comparison algorithms some will contend identification of an unknown compound from its mass. This course is not instrumentspecific and is suitable for anyone involved in mass spectrometry, from the analysts who wants to obtain good spectral data to the lab manager who needs to understand spectral interpretation in order to validate that data.

Molecular weight divided by the charge on this protein all proteins are sorted based on a mass to charge ratio mz 12. Such an approach is very useful for the interpretation of the mass spectra of. Mass ranges of 10 to daltons are common to gcms systems today. Not all compounds will give a mass spectrum as the compound of interest may not ionise. Pdf download interpretation of mass spectra, by fred w. Data system mass detector analyzer vacuum system source inlet region more precisely mass spectrometry determines the mass of a molecule. Interpretation of mass spectra interpretation of ms.

Introduction to mass spectral interpretation by robert kobelski each mass spectrum contains a wealth of information. 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. You need to understand mass spec well for it to be of good use. Nist epanih mass spectral library nist 05 and nist mass spectral search program version 2. In person analysis and interpretation of mass spectral data. In this application, isobaric masses are differentiated and. David sparkman has been a member of asms since 1977 and the acs since 1967. Mass spectrometry ms is an analytical technique that measures the mass tocharge ratio of ions. How to quickly solve spectrometry problems this tutorial is meant to streamline the process by cutting out redundancies and saving time. In the mass spectrum, the heaviest ion the one with the greatest mz value is likely to be the molecular ion.