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1、现代有机质谱概论,杨松成仪器测试分析中心,Outline,Introduction Instrument of OMS Tandem Technology Main Application Most New Advances,Modern Organic Mass Spectrometry(OMS)Molecular Mass Spectrometry,OMS is a basic and high-technical science In which,physics,electronics and computer science were applied to study physical
2、 and chemical character of organic molecules,Mass Spectrometry had its origin in early last century Application of organic mass spectrometry for chemical analysis occurred in early 1940s,Quantitative analysis of hydrocarbon mixtures(9)produced in catalytic crackers,Methods require time,Fractional di
3、stillation,refractive index 200 hoursOrganic mass spectrometry one hour or more,Beginning in the 1950s,chemists have used commercial organic mass spectrometer for identification and structural elucidation of a wide variety of organic compounds,The use of the MS combined with the NMR IR and UV revolu
4、tionized the way organic chemists went about identifying and determining the structure of organic molecules,Organic Mass Spectrometry,Determine molecular weight Elucidate structure of organic molecule Identify unknown compounds Quantify known materials Accuracy,sensitive and rapid,OMS has been a pow
5、erful analytical tool in modern structure chemistry and analytical chemistry,Before the middle of the 1970s OMS could only analyze organic molecules with molecular weight below 1000 Da,1974 Plasma Desorption Mass Spectrometry PD-MS1981 Fast Atom Bombardment Mass Spectrometry FAB-MS1988 Electrospray
6、Ionization Mass Spectrometry ESI-MS1988 Matrix-assisted Laser Desorption Ionization Time of Flight Mass Spectrometry MALDI-TOF-MS,Outline,Introduction Instrument of OMS Tandem Technology Main Application Most New Advances,Organic Mass Spectrometry is a name for a collection of techniques used to mea
7、sure the masses of organic ions and their abundance in the gas phase,Main components of OMS,Ion Sources Mass Analyzer Main Fundamentals of OMS,Ion sources for organic mass spectrometry,Basic type Name and acronym Ionizing agent,Gas phase Electron impact(EI)Energetic electrons Chemical ionization(CI)
8、Reagent gaseous ions Field ionization(FI)High-potential electrodeDesorption Field desorption(FD)High-potential electrode Electrospray ionization(ESI)High electrical field Matrix-assisted laser desorption ionization(MALDI)Laser beam Plasma desorption(PD)Fission fragments from 252Cf Fast atom bombardm
9、ent(FAB)Energetic atomic beam Secondary ion mass spectrometry(SIMS)Energetic beam of ion Thermospray ionization(TS)High temperature,Gas phase sources:the sample is first vaporized and then ionizedDesorption sources:the sample in a solid or liquid state is converted directly into gaseous ions,MALDI-T
10、OF-MS of rhEGF,Main components of OMS,Ion Sources Mass Analyzer Main Specification of OMS,Mass Analyzer,Magnetic Sector Analyzer Quadrupole Mass Analyzer Ion Trap Mass Analyzer Time of Flight Mass Analyzer FT-ICR Mass analyzer,Reverse Geometry Double Focusing Mass Spectrometer,V Kinetic energy of th
11、e ion E Potential field applied across the plate,Ion Trap Mass Analyzer,Time of Flight Mass Analyzer,Fourier Transform Ion Cyclotron Resonance Mass Analyzer,Schematic Diagram of the ICR Cell,Character of FT-ICR-MS,Ultra-high resolution Ultimate mass accurate Enhances dynamic range The power of M S,n
12、,Main components of OMS,Ion Sources Mass Analyzer Main Fundamentals of OMS,Main Fundamentals of OMS,Mass Definition Mass Range Resolution Mass Accuracy Sensitivity,Mass Accuracy,Outline,Introduction Instrument of OMS Tandem Technology Main Application Most New Advances,Qualitative Analysis,Pure subs
13、tance identification Mixture Separation identification,Mass spectrometry is a powerful analytical tool for identification of pure organic molecules,Tandem Technology,Gas Chromatography-Mass Spectrometry GC-MS Liquid Chromatography-Mass Spectrometry LC-MS Capillary Electrophoreses-Mass Spectrometry C
14、E-MS Tandem Mass Spectrometry MS/MS,Liquid Chromatography-Mass Spectrometry,LC-MS interface has been studied for more than 1/4 century About 25 kinds of LC-MS interface has been reported,Before API,attempts were made to couple HPLC analysis with a variety of mass spectrometry techniques.But these at
15、tempts were some success.The great advantages of API MS is its ready compatibility with separation techniques such as HPLC and CE.,Atmosphere Pressure Ionization(API),Atmosphere pressure chemical ionization(APCI)is mainly used for HPLC-MS.Electrospray ionization(ESI)is used for HPLC-MS and CE-MS,HPL
16、C APCI-MS,LC-MS is now a mature technique,Innovation in chromatographic part,Short HPLC column(10 50 mm)Micro packing materials(5,3.5,1.7 um),1 D HPLC-MS 2 D HPLC-MS,1 D LC Injection,1 D LC-MS,Schematics of 2D Capillary/Nano LC,Capillary Electrophoresis Mass Spectrometry,Tandem Mass Spectrometry,197
17、8 Mclafferty Cornell University1978 Cook Purdue University,Reversed geometry double-focusing mass spectrometer,MIKES(Mass analyzed ion kinetic energy spectrometry),1979 Yost,Triple Stage Quadrupole Mass Spectrometer(TSQ-MS),Tandem Mass Spectrometry(MS/MS),C I D of Peptide,Mass Spectrometry used in B
18、iomedicine,Outline,Introduction Instrument of OMS Tandem Technology Main Application Most New Advances,Identification of Pure Organic Compounds,Molecular weight from mass spectrometry Molecular formulas from exact molecular weight Molecular formulas from isotopic ratios Structure information from fr
19、agmentation patters Compound identification from comparison spectra Computerized library search systems,Analysis of mixtures by tandem methods,Gas Chromatography-Mass Spectrometry GC-MS Liquid Chromatography-Mass Spectrometry LC-MS Capillary Electrophoreses-Mass Spectrometry CE-MS Tandem Mass Spectr
20、ometry MS/MS,Mass spectrometry is now applied to all the disciplines associated with organic molecules,Main application of mass spectrometry in biomedicine,Elucidation of the structure of organic and biological molecules Determination of the molecular weight of peptides,proteins and oligonucleotides
21、 Determination of amiono acid sequences of peptides and proteins Identification of proteins Determination of protein mutation Determination of-SH and disulfide bond in proteins Determination of post-translational modification of proteins Study on high structure of proteins Study on non-covalent bond
22、 interaction between biomolecules Mass Spectrometry-based proteomics,Oligonucleotides sequencing SNP determination Study on drug metabolism New drug discovery by proteomics approach study on drug mechanisms by proteomics approach Mass spectrometry-based metabonomics Diagnosis of metabolism disease F
23、orensic application Determination of pesticides residues in food Testing for the presence of drugs in blood and urine in thoroughbred racing horses and in Olympic athletes Analysis of aerosol particles Detection and identification of microorganism Modernization research of Chinese traditional herbs,
24、Outline,Introduction Instrument of OMS Tandem Technology Main Application Most New Advances,Hybrid Tandem Mass Spectrometry and New Mass Analyzer,Quadrupole-Time of Flight Mass Spectromertry(Q-TOF MS)Orbitrap Analyzer and LTQ Obitrap Mass Spectrometry Ion Trap Time of Flight Mass Spectrometry,Waters
25、 company,Waters Synapt G2,High resolution over 40,000 FWHM Linear dynamic range of up to 105 Exact mass 1 ppm RMS UPLC compatible acquisition rates 20 spectra/sec,Thermo Fisher company,Orbitrap Analyzer,UPLC-MS,HPLC(High performance liquid chromatography)UPLC(Ultra performance liquid chromatography)
26、,Van Deemter plot,Comparison of HPLC and UPLC for a ginger root exact,Mass Spectrometry from Proteomics to Metabolomics Lipidomics MADI Imaging Microorganisms Identification,Principle of MALDI Imaging Mass Spectrometry,MALDI Molecular Imager,Laser-technology(Smartbeam)is the key technology for MALDI
27、 imaging,Resolution:achieve a spatial resolution of 10 m Speed:acquire spectra with 200 Hz laser frequency Precision:x y-stage precision is 5 m,MALDI imaging of a 12 m coronal mouse brain section,a)Photomicrograph of histologically stained Coronal mouse brain section 1.Cerebral cortex 2.Corpus callo
28、sum 3.Striatum,Characterization of human gastric cancer by MALDI Imaging,A Histologically stained reference sectionB MALDI imaging experiment Left:two signals for non-tumor area Right:red signal for the tumor area,blue signal for the non-tumor area,Pseudo gel-view of mass spectra from imaging runs,M
29、ALDI Biotyper,Microorganism identification and classification Identify microorganisms in minutes in one simple step,The proteomic fingerpring,Disclose bacterias identity by its own unique protein composition,Unknownmicrorganism,Select a colony,Smear a thin-layer ontoa MALDI target plate,Generate MALDI-TOFprofile spectrum,BioTyperData interpretation,Identified species,?,Bacillus globigii,MALDI biotyper workflow,谢 谢！,
