Mass spectral interpretation pdf

Mar 27, 2015 general steps in mass spectral interpretation 10. 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. Introduction to mass spectrometry wiley online books. This paper covers the basics of mass spectrometry instrumentation and introduces the interpretation of mass spectra. My thanks are extended to the staff of my facility n. Interpretation of mass spectra interpretation of ms. The method was set to analyze the top 10 most intense ions from the survey scan and a dynamic exclusion was enabled for 15 s.

It is also called as positive ion spectra or line spectra. Mass spectrometry works by ionizing chemical compounds to generate. The leading scientist in this field was fred mclafferty who together with frantisek turecek has written a very famous text book. A mass range of 1002000 mz and a normalized collision energy of 30 was used for the survey scans. 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.

Ei spectra are rich in fragments thus useful in structure determination thro interpretation. The separation of pnp isomers was not optimized with one set of gc conditions. Take your mass spec knowledge and skills to the next level with mass s selfpaced courses. Software tools that calculate glycopeptide composition from msonly data will not be summarized in detail. For larger molecules, it is common to see higher charge states, such as z 2 or z 3. 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. Flock for their efforts and to the staff of the local libraries for their friendly support. 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. With the multiple charging phenomena displayed in electrospray spectra how does one calculate the mass of a compound. 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.

The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be analysed. Mass spectra is a plot of relative abundance against mass tocharge ratio. Mass spectroscopy mass spectroscopy is a technique causing the formation of the gaseous ions with or without fragmentation. 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. Chapter 2 fragmentation and interpretation of spectra 2. It is well written and he also stresses pitfalls students routinely make in analysis. Nitrogen has an even atomic mass but bonds with three other atoms in its most stable form. It is an excellent source of information for the mass spec novice. 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. 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. Examine spectrum for peak clusters of characteristic isotopic patterns. Mass spectrometry a textbook, problems and solutions website. Most processes are very rapid, occurring within a few nano or microseconds. His book offers a balanced mixture of practiceoriented information and theoretical.

For the analytical chemist, a mass spectrum is useful for two applications. Microsoft word guide to interpretation of mass spectra. This information is used to elucidate the chemical structures of molecules, such as pesticides or peptides. Terrence lees book title, a beginners guide to mass spectral interpretation is quite accurate. Introduction to mass spectral interpretation by robert kobelski each mass spectrum contains a wealth of information. Approaches that analyze deglycosylated peptides using proteomics approaches are not included. The mass to charge ratio mz is used to describe ions observed in mass spectrometry. Mass spectrometry is used in many different fields and is applied to pure samples as well as complex mixtures. The expanding role of mass spectrometry in biotechnology 2nd edition. Lcms fundamentals and applications mass spectral intrepretation peptide and protein characterization optimization and validation of lcms methods. Parent ion may be absent aliphatic alcohols, nitrites, nitrates, nitro.

Gas chromatographymass spectrometry gc ms interpretation of ei spectra jeremy keirsey ccic msp. This rule is a result of nitrogens unique property. Mass ranges of 10 to daltons are common to gcms systems today. Oct 05, 2007 he is the author of mass spectrometry desk reference. Mass spectral interpretation is the method employed to identify the chemical formula, characteristic fragment patterns and possible fragment ions from the mass spectra. 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. The chapter includes an introduction to the main ionisation techniques in mass spectrometry and the way the resulting fragments can be. Isotopic percentage and nominal mass calculation are also. The book emphasizes the use of this important analytical technique in many different. 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. Pdf download interpretation of mass spectra, by fred w.

Nistepanih mass spectral library nist 05 and search. Nistepanih mass spectral library nist 17 and nist mass. Nominal mw will be an odd number if the compound also contains an odd. Jul 21, 2017 mass defect is associated with the binding energy of the nucleus. Molecular weight divided by the charge on this protein all proteins are sorted based on a mass to charge ratio mz 12. How to quickly solve spectrometry problems this tutorial is meant to streamline the process by cutting out redundancies and saving time. Interpretation of a mass spectrum is often compared to doing a jigsaw puzzle. 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. This peak if it appears will be the highest mass peak in the spectrum, except for isotope peaks.

Stein, technical leader william wallace, group leader evaluation. The following is a summary of software tools for interpretation of intact glycopeptide mass spectral data. Mass spectral interpretation using the rule of author. Using the molecular ion to find the relative formula mass. In mass spectrometry ms, the obvious concern is the actual masses of the atoms, molecules, or fragment thereof. This book consists of nine chapters and begins with a historical overview of mass spectrometry. For the fourth in the analytical chemistry series, we turn to mass spectrometry. The results are typically presented as a mass spectrum, a plot of intensity as a function of the mass tocharge ratio. Sauerwein to use a large set of electron ionization mass spectra from the nistepanih mass spectral library is also gratefully acknowledged. Mass spectral fragments of common hydrocarbons mass spectral peaks can be identified to have originated from the fragmentation of specific hydrocarbon sources including. Mass spectrum is the balance of a series of competing and consecutive reactions 5456. Data system mass detector analyzer vacuum system source inlet region more precisely mass spectrometry determines the mass of a molecule. Typical mass spectrometry research focuses on the formation of gas phase ions, the chemistry of ions, and applications of mass spectrometry.

It has contributed to numerous discoveries in chemistry, physics and biochemistry. Mass spectrometry of fatty acids a beginners guide part 1. You need to understand mass spec well for it to be of good use. 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. Starting from the very principles of gasphase ion chemistry, isotopic composition, and accurate mass, jurgen h. Nistepanih mass spectral library nist 17 and nist mass spectral search program version 2. 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. The ionized molecule often fragments into smaller ionsradicals.

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. The survey scans were acquired in the orbitrap mass analyzer operating at 120,000 fwhm resolving power. For singlycharged species z 1, the observed mass corresponds to the monoisotopic mass. The guide arose from discussions held at the vam mass spectrometry. Present fundamental concepts regarding mass spectral interpretation objectives at the end of this section you should be able to. Ms interpretation general interpretation strategies. In heterolytic cleavage, an electron pair moves together to the charged atom. Sooner you get guide interpretation of mass spectra, by fred w. It will be your resort to maintain downloading guide interpretation of mass spectra, by fred w. Such an approach is very useful for the interpretation of the mass spectra of. In person analysis and interpretation of mass spectral data. Interpreting electrospray mass spectra an ionsource.

Aims and scope of mass spectrometry a textbook mass spectrometry today is an indispensable tool in chemistry and life sciences. A few compounds have mass spectra which dont contain a molecular ion peak, because all the molecular ions break into fragments. Do not think of this as an algorithm but as second nature. In the mass spectrum, the heaviest ion the one with the greatest mz value is likely to be the molecular ion. In mass spectrometry, one generates ions from a sample to be analyzed. Mass spectrometry and interpreting mass spectra compound. Please create your bookmark, if you are interested in learning about mass spectrometry, mass spectral interpretation, instrumentation, and the full range of ionization methods. Comparative analysis of mass spectral matching for confident. It is a fundamental property of the nucleus and the principle behind nuclear energy. Mass spectral determination of fasting tear glucose concentrations in nondiabetic volunteers, justin t. Mass spectrometry ms is an analytical technique that measures the mass tocharge ratio of ions.

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. A beginners guide to mass spectral interpretation 19 feb 2014. Please list your special interest on the registration form below. Isotopes hold a special place not only in ms but also, in general terms, in chemistry and physics. He has developed and taught 10 sessions of an interactive web course on mass spectral interpretation over the past 4 years.

Version see revision notice the nist mass spectrometry data center stephen e. If good inferences could be made, use the remainder of the mass spectrum to try to elucidate structural features or isomerism. Pdf a beginners guide to mass spectral interpretation. Learn simple and easytounderstand lcms approaches for structure identification of metabolites, impurities, natural products, and biomolecules. Computerization of mass spectral data is also discussed. This website offers problems and solutions corresponding to each chapter of mass spectrometry a textbook, 3rd edition. Allows specific compound identification structural elucidation via spectral interpretation. Other atoms that have even molecular weights like carbon, oxygen, and. If other spectroscopic data is available analyze fully confirm inferences from table 1 and presence of elements in table 2. Mass spectrometry ms is a mainstream chemical analysis technique in the twentyfirst century. In this application, isobaric masses are differentiated and. Aists spectral database, which includes 1 h and c nmr spectra, as well as ir, uvvis, and mass spectra.

David sparkman has been a member of asms since 1977 and the acs since 1967. A beginners guide to mass spectral interpretation terrence. Mclafferty sooner you get guide interpretation of mass spectra, by fred w. Request pdf mass spectral interpretation the identification of metabolites is an integral part of the drug discovery and development process. The first mass spectral measurements were undertaken by j. Mass spectrometry mass spectrometry is the most accurate method for determining the molecular mass of the compound and its elemental composition. 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. Nist epanih mass spectral library nist 05 and nist mass spectral search program version 2.

Not all compounds will give a mass spectrum as the compound of interest may not ionise. Gross leads through the design of all types of mass analyzers and ionization methods to mass spectral interpretation and coupling techniques. Lecture notes in eimass spectrometry by torben lund. These strategies are what i noticed when i was completing the practice problems. 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. 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. From spectra, the mass of the molecular ion and fragments are used to determine the elemental composition or isotopic signature of a compound.

The number of hits may also be reduced by taking an accurately measured isotope pattern of the ion into consideration. While this is less useful in a more advanced spectroscopy. 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. Interpretation of mass spectra of organic compounds.

The 2017 version of the nistepanih mass spectral library nist 17 contains four mass spectral libraries and a library of retention index rigc method. 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. The number of compounds with gc methodsri library in the ei ms library mainlib is 72,361. 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. Protein sequencing and identification with mass spectrometry. It is only an introduction and interested readers are encouraged to consult more specialized books and journal articles for additional details. Comprehensive structural characterization of phenolics in. 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. Anzor mikaia, principal vladimir zaikin ei damo zhu ei. It is commonly used for the identification of organic compounds from electron ionization mass. Shows you how to get the information out of a mass spectrum and use it to help suggest the identity of an unidentified molecule. 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. Mass spectrometry is a wideranging analytical technique, which involves the production.