Mass Spectrometry Mass Spec. .

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Prologue to Mass SpectrometryIonization MethodsMass AnalyzerFragmentation and MS InterpretationHyphenated MS Techniques. Layout. By James Crawford. How do two individuals with distinctive dialects correspond with one another?. At that point, by what means would I be able to make up for lost time, Ms.?. Substance Identification. Examination of Physical PropertiesBoiling PointMelting PointDensityOptical rotationAppearanceOdor.
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Mass Spectrometry (Mass Spec.) Prof. Yonghai Chai School of Chemistry & Materials Science For Bilingual Chemistry Education

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OUTLINE Introduction to Mass Spectrometry Ionization Methods Mass Analyzer Fragmentation and MS Interpretation Hyphenated MS Techniques

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By James Crawford How do two individuals with various dialects speak with each other? At that point, how might I get up to speed, Ms.?

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Chemical Identification Comparison of Physical Properties Boiling Point Melting Point Density Optical pivot Appearance Odor Elemental Analysis Burn the compound and measure the measures of CO 2 , H 2 O and different parts that are delivered to decide the observational recipe

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Spectroscopic Methods for Structure Determination Ultraviolet-Visible (UV/Vis) spectroscopy: assurance of arrangements of move metal particles and exceedingly conjugated natural mixes Infrared (IR) spectroscopy: Functional gatherings Mass spectrometry (MS): Molecular mass and equation and structure data Nuclear attractive reverberation (NMR) spectroscopy: Map of carbon-hydrogen system

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Definition of Mass Spectrometry Mass spectrometry (MS) : An expository procedure by utilizing mass spectrometry for the assurance of the piece of a specimen or atom and explanation of the synthetic structures of atoms, for example, peptides and other concoction mixes. Mass spectrometry has been depicted as the littlest scale on the planet, not in light of the mass spectrometer\'s size but rather as a result of the span of what it weighs - atoms.

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Timeline for MS Development 1897 Early Mass Spectrometry 1919 The perception of isotopes utilizing mass spectrometry 1934 Double Focusing Analyzer 1939 Accelerator Mass Spectrometry 1946 Time-of-Flight Mass Spectrometry 1947 Preparative Mass Spectrometry 1949 Ion Cyclotron Resonance (ICR) Reverse Geometry Double centering MS 1953 Quadrupole Analyzers Joseph John Thomson " In acknowledgment of the immense benefits of his hypothetical and exploratory examinations on the conduction of power by gasses." 1906 Nobel Prize "At first there were not very many who put stock in the presence of these bodies littler than iotas. I was even told long a short time later by a recognized physicist who had been available at my [1897] address at the Royal Institution that he thought I had been \'pulling their legs." Cited from: of J.J. Thomson\'s third mass spectrometer.

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Continuation of Timeline 1956 Gas Chromatography Mass Spectrometry (GC/MS) Identifying Organic Compounds with Mass Spectrometry 1962 Mass Spectrometry Imaging 1966 Chemical Ionization 1966 Peptide Sequencing 1966 Tandem Mass Spectrometry 1966 Metabolomics 1968 Electrospray Ionization Collision Induced Dissociation 1969 Field Desorption-MS of Organic Molecule Francis William Aston "For his revelation, by method for his mass spectrograph, of isotopes, in a substantial number of non-radioactive components, and for his articulation of the entire number rule." Mass spectrometry of isotopes 1922 Nobel Prize Cited from:

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Continuation of Timeline 1974 Fourier Transform Ion Cyclotron Resonance 1974 Extra-Terrestrial Mass Spectrometry 1975 Atmospheric Pressure Chemical Ionization (APCI) 1976 Californium-252 Plasma Desorption MS 1978 GC-C-IRMS 1978 Triple Quadrupole Mass Analyzer 1980 Inductively Coupled Plasma MS 1981 Matrix-Assisted Desorption Ionization 1984 Quadrupole/Time-Of-Flight Mass Analyzer 1985 Matrix-Assisted Laser Desorption Ionization (MALDI) Wolfgang Paul Hans Georg Dehmelt "For the improvement of the particle trap system." 1989 Nobel prize Cited from:

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Continuation of Timeline ESI 1987 Soft Laser Desorption of Proteins 1989 ESI on Biomolecules 1989 Monitoring Enzyme Reactions with ESI-MS 1990 Protein Conformational Changes with ESI-MS 1990 Clinical Mass Spectrometry 1991 MALDI Post-Source Decay 1991 Non-covalent Interactions with ESI 1992 Low Level Peptide Analysis 1993 Oligonucleotide Ladder Sequencing 1993 Protein Mass Mapping 1996 Intact Virus Analyses John B. Fenn MALDI Koichi Tanaka "For the improvement of delicate desorption ionization techniques for mass spectrometric investigations of natural macromolecules." Cited from:

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Continuation of Timeline 1998 Electron Capture Dissociation (ECD) 1999 Nanostructure Desorption/Ionization Quantitative Proteomics and Metabolomics with Isotope Labels 2000 Orbitrap 2004 Desorption Electrospray Ionization (DESI) 2004 Electron Transfer Dissociation (ETD) 2005 Direct Analysis in Real Time (DART) Fred W. McLafferty Alfred O.C. Nier Alan G. Marshall Klaus Biemann R. Graham Cooks Donald F. Chase Catherine Fenselau Franz Hillenkamp Carol V. Robinson Michael Karas Malcolm Dole Brian T. Chait Cited from:

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What data can be resolved? Sub-atomic weight Molecular recipe (HRMS) Structure (from discontinuity unique mark) Isotopic consolidation/dissemination Protein succession (MS-MS)

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Schematic Mass Spectrometer � �品 检测器 离子源 质量分析器 数据分析处理器

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What\'s in a Mass Spectrum Mass-to-charge proportions of a particle or its piece are charted or classified by relative plenitude Fragment Ions Fragment Ions: got from sub-atomic particle or higher weight sections

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Applications Biomolecule portrayal Pharmaceutical examination Proteins and peptides Oligonucleotides Paleoclimatology and Archeology Forensic investigation/clinical Environmental examination Pesticides on nourishments Soil and groundwater pollution Paleotemperature O 16 and O 18 foraminifera

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Relative Abundance of Isotopes Atomic weight of a component is a weighted normal of the actually happening isotopes.

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Isotopic Ratio from the Spectra Mass spec. can be utilized to gauge the isotopic proportions

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Continuation of Isotopes Chlorine ( 35 Cl to 37 Cl is 3:1, give M + 2)

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Ionization Methods Electron bomb Ionization ( 电子轰击离子化 ) EI Chemical Ionization ( 化学电离 ) CI Field ionization ( 场电离 ) FI Matrix Assisted Laser Desorption Ionization ( 基质协助的激光解吸 ) MALDI Fast particle barrage ( 快原子轰击 ) FAB Electro Spray Ionization ( 电喷雾 ) ESI

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( M - R 2 ) + Mass Spectrum ( M - R 1 ) + M + ( M - R 3 ) + Electron Bomb Ionization ( EI ) Sample is warmed and empowered by a light emission, typically gives a sub-atomic particle (M+) and a considerable measure of pieces 。

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Electron Bomb Ionization ( EI )

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Properties of EI Hard ionization Gas-stage particles enter source through warmed test or GC segment 70 eV electrons besiege atoms framing M+* particles that section in novel reproducible approach to shape a gathering of section particles EI spectra can be coordinated to library sexually transmitted diseases CI (delicate ionization) Higher weight of methane spilled into the source (mtorr) Reagent particles exchange proton to analyte

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Chemical Ionization (CI) Electron ionization prompts to fracture of the sub-atomic particle, which in some cases keeps its location. Synthetic ionization (CI): A strategy that produces particles with minimal overabundance vitality. Subsequently this strategy displays the upside of yielding a range with less discontinuity in which the atomic species is effectively perceived. Therefore, substance ionization is reciprocal to electron ionization.

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Chemical Ionization (CI)

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Advantages Parent Ion Interface to GC Insoluble Samples Disadvantages No Fragment Library Need Volatile Sample Need Thermal Stability Quantitation Difficult Low Mass Compounds (<1000 amu) Solids Probe Requires Skilled Operator Properties of CI

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+ 阳极 + d <1mm 阴极 Field ionization (FI) Field ionization (FI) is a strategy that utilizations exceptionally solid electric fields to create particles from gas-stage atoms .

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Field ionization (FI)

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Matrix Assisted Laser Desorption Ionization (MALDI) test is co-solidified with a lattice and afterward illuminated with laser. MALDI is accomplished in two stages. In the initial step, the compound to be broke down is broken up in a dissolvable containing in arrangement little natural particles, called the framework. The second step happens under vacuum conditions inside the wellspring of the mass spectrometer.

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Properties of MALDI Good dissolvability Vapor weight must be adequately low to keep up vacuum conditions Viscosity must permit dissemination of the analyte from the mass to the surface Polar : to solvate and separate preformed particle Less Sensitive to Salts Lower PRACTICAL identification limits Easier to decipher spectra (less different charges) Quick and simple Higher mass recognition Higher Throughput (>1000 tests every hour)

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MALDI mass spectrometry has turned into an intense scientific apparatus for both engineered polymers and biopolymers . Standard of MALDI

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Fast molecule assault ( FAB) Softer than EI and CI. Particles are created by assault with substantial iotas. Gives (M+H) + particles and litle discontinuity. Useful for more polar mixes. Ar + e Ar + quickening (5-15 KeV) Ar+ + Ar + Ar + quick moderate + 8 KeV quick moderate

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Advantages Parent Ion High Mass Compounds (10,000 amu) Thermally Labile Compounds (R.T.) Disadvantages No Fragment Library Solubility in Matrix (MNBA, Glycerol) Quantitation Difficu

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