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GC-MS a new integrated technique that uses combined advances of GC-MS that should improve the time and efficiency of the result.


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Gas Chromatography & Mass Spectroscopy Seminar By : Seminar Guide: Nikhil A. Khisti Prof. Deshpande (M.Pharm 1 st Sem.) (Pharma. Chemistry) :

1 23-Nov-11 1 Gas Chromatography & Mass Spectroscopy Seminar By : Seminar Guide: Nikhil A. Khisti Prof. Deshpande (M.Pharm 1 st Sem.) (Pharma. Chemistry) Gas Chromatography & Mass spectroscopy Seminar By : Nikhil A. Khisti Shital S.Bhandari Department of Pharmaceutical Chemistry AISSMS College of Pharmacy Pune-411038


2 CONTENTS What is gas chromatography ? What is mass spectroscopy ? Interfacing gas chromatography with mass spectrometry History Instrumentation Application References 23-Nov-11 2

What is gas chromatography ? [3]:

3 What is gas chromatography ? [3] Gas chromatography is a physical separation technique applicable to volatile and thermally stable compounds which are difficult to separate and analyze. It consist of a mobile gas phase and stationary liquid phase that is coated on a solid. 23-Nov-11 3

What is mass spectroscopy? [3]:

4 What is mass spectroscopy? [3] Mass spectroscopy is an analytical technique capable of providing information about the structure of inorganic, organic & biological molecules; the qualitative & quantitative composition of complex mixture. In this technique molecules are bombarded with a beam of energetic electrons, to form positively charged ions which are further sorted according to their mass to charge ratio to record their masses and relative abundances. 23-Nov-11 4

History [9]:

5 23-Nov-11 5 History [9] In December 1955, Roland S. Gohlke and Fred W. McLafferty coupled a home made gas chromatograph to a research time-of-flight mass spectrometer constructed by W. C. Wiley, I. H. McLaren, and D. B. Harrington. The development of affordable and miniaturized computers has helped in the simplification of the use of this instrument, as well as allowed great improvements in the amount of time it takes to analyze a sample 23-Nov-11 5

GC-MS System [4]:

6 23-Nov-11 6 GC-MS System [4] Gas chromatography-mass spectroscopy (GC-MS) is one of the so-called hyphenated analytical techniques . As the name implies, it is actually two techniques that are combined to form a single method of analyzing mixtures of chemicals. Gas chromatography separates the components of a mixture and mass spectroscopy characterizes each of the components individually. By combining the two techniques, an analytical chemist can both qualitatively and quantitatively evaluate a solution containing a number of chemicals. 23-Nov-11 6

Why Gas Chromatography/Mass Spectrometry? [16]:

7 23-Nov-11 7 Why Gas Chromatography/Mass Spectrometry? [16] Like a good marriage, both GC & MS bring something to their union. GC can separate volatile and semi volatile compounds with great resolution, but it cannot identify them.MS can provide detailed structural information on most compounds such that they can be exactly identified, but it cannot readily separate them. GC & MS are, in many ways, highly compatible techniques. The main aim of an interfacing arrangement is to operate both GC & MS without degrading the performance of either instrument. 23-Nov-11 7

Advantages [1]:

8 23-Nov-11 8 Advantages [1] Enhanced sensitivity Speed Dynamic range Molecular weight Elemental composition (low MW with high resolution instrument) Structural information (hard ionization) 23-Nov-11 8

How does it work? [16]:

9 23-Nov-11 9 How does it work? [16] A gas chromatograph separate different types of molecules, based on their chemical properties. Resulting in each type emerging from the column in a defined sequence. The molecules would then enter the mass spectrometer, which would evaluate and identify them by breaking each one into ionized fragments and detecting these fragments using their charge-to-mass ratio. This produced a unique profile of each compound that could be converted into a digital signal and transmitted to computer 23-Nov-11 9

GC MS Instrument [9]:

10 23-Nov-11 10 GC MS Instrument [9] 23-Nov-11 10 The insides of the GC-MS, with the column of the gas chromatograph in the oven on the right.

Schematic Diagram [3]:

11 Schematic Diagram [3] 23-Nov-11 11

Instrumentation [4]:

12 23-Nov-11 12 Instrumentation [4] Parts of a Gas Chromatography: 1. Carrier Gas (N2,He) 2. Injector (Loop Inj. ,Stop flow) 3. Oven 4. Column (FSOT,SCOT) Interface between GC and MS: (Effusion, Jet/Orifice Sp) Parts of a Mass Spectroscopy: 3. Source (EI,FI,CI) 4. Mass analyzer (Quadruple Filter.) 5. Detector (electron multiplier tube) 23-Nov-11 12

Carrier gases [3]:

13 Carrier gases [3] Helium, Nitrogen , Argon ,Hydrogen Ideally The Carrier gas should be : * Inert * easily available * non explosive * highly pure * Suitable for detector/Sample 23-Nov-11 13

Injector [1]:

14 23-Nov-11 14 Injector [1] A GC syringe penetrates a septum to inject sample into the vaporization camber Instant vaporization of the sample, 280  C Carrier gas transports the sample into the head of the column Purge valve controls the fraction of sample that enters the column 23-Nov-11 14

Oven [3]:

15 23-Nov-11 15 Oven [3] More constant peak width Better sensitivity for components that are retained longer Much better chromatographic resolution Peak refocusing at head of column 23-Nov-11 15

Open Tubular Capillary Column:

16 23-Nov-11 16 Open Tubular Capillary Column 23-Nov-11 16 0.32 mm ID Liquid Stationary phase Mobile phase (Helium) flowing at 1 mL/min 15-60 m in length 0.1-5 m m

FSOT columns [3]:

17 23-Nov-11 17 FSOT columns [3] Column length -10-100 m Inner Diameter - 0.1-0.53 mm Efficiency (Plates/m) - 2000-4000 Total No. of Plates - 20-400 x 10 3 Relative Speed -High Chemical Inertness -Inert for many Chemicals Flexibility -More Materials Used: Poly (phenyl methyl di methyl) siloxane (10% phenyl) Poly (phenyl methyl) siloxane (50% phenyl) Poly ethylene glycol (polar) Poly dimethyl siloxane (non-polar) 23-Nov-11 17

Interface [16]:

18 Interface [16] Transports the effluent from gas chromatograph to mass spectrometer Analyte must not condense in interface Analyte may not decompose before entering the mass spectrometer ion source The gas load entering the ion source must be within pumping capacity of the mass spectrometer

Electron Impact [2] :

19 23-Nov-11 19 Electron Impact [2] EI (hard ionization) Gas-phase molecules enter source through heated probe or GC column 70 eV electrons bombard molecules forming M+* ions that fragment in unique reproducible way to form a collection of fragment ions EI spectra can be matched to library standards 23-Nov-11 19

PowerPoint Presentation:

20 23-Nov-11 20 23-Nov-11 20 To mass analyzer filament 70 eV e- anode repeller Acceleration slits GC column EI Source Under high vacuum [2]

Quadruple Mass Ion Filter [1]:

21 23-Nov-11 21 Quadruple Mass Ion Filter [1] 23-Nov-11 21

Steps in GC/MS analysis [4] :

22 Steps in GC/MS analysis [4] Sample preparation Derivatisation Injection GC separation Ion Formation MS Detection Scanning 23-Nov-11 22

GC-MS Video :

GC-MS Video 23-Nov-11 23 23 23-Nov-11 23


24 23-Nov-11 24 APPLICATIONS 23-Nov-11 24

PowerPoint Presentation:

25 Pharmaceuticals Pesticides Perfumery Foods Petroleum Polymers Environmental analysis 23-Nov-11 25 Biomedical Criminal forensics Textiles Clinical toxicology Explosive investigation Doping in Sport Astrochemistry

Pharmaceuticals [11] :

26 Pharmaceuticals [11] separation and identification of degradation products of organic & organometallics making the elucidation of their structures. Routine analysis of substances present in minute quantities Molecular weight of pure drug To identify organic materials such as resins, fats & waxes from their chemical composition. 23-Nov-11 26

Pesticide [12]:

27 Pesticide [12] Identification of agrochemicals. Quantitative determination of pesticide residues in food water, etc. Quantization & conformation of organophosphorus pesticides in apple extract. Rapid screening and conformational analysis of residual pesticides in agricultural samples. 23-Nov-11 27

Perfumery & essential oils [13] :

28 Perfumery & essential oils [13] Perfumery & essential oils are very complex compound of natural origin. Each compound can contain 50 to 60 constituents or more which can be separated only by a high resolution capillary column. MS is the only means of identifying these components since it is practically impossible to get standards for them 23-Nov-11 28

Foods [14] :

29 Foods [14] Analysis of flavoring compounds. Analysis of residual solvents in packing materials. Determination of residual pesticides in foods. In analysis of food, the separation & identification of lipids, proteins, carbohydrates, preservatives, colorants & texture modifiers. To analyze the dairy products for aldehydes & ketones, fatty acids & milk sugars. Analysis & Detection of 3-monochloropropane-1,2-diol in food 23-Nov-11 29

Textiles [15]:

30 Textiles [15] GC-MS is a very valuable tool for the detection and estimation of banned amines in dyes on the garments. Any possible banned amine in the dyes is extracted from the garment and subjected to GC-MS analysis. 23-Nov-11 30

Clinical toxicology [16]:

31 Clinical toxicology [16] The applicability of GC-MS for use in clinical toxicology lab was demonstrated in 1970s. One of the earliest clinical application was by Althaus who in 1970 identified propoxyphene and metabolites as agent responsible for coma in patient admitted to local hospital. Identification and confirmation of underivatized drug from extracts of urine or serum . Drug screening using GC/MS e.g. caffeine, Codeine , Methadone, Monoacetyl Morphine 23-Nov-11 31

Explosive investigation [17] :

32 Explosive investigation [17] GC-MS can also be used in airport security to detect substances in luggage or on human beings. Explosive detection systems have become a part of all airports. 23-Nov-11 32

Doping in Sport Symposium Proceedings [18] :

33 Doping in Sport Symposium Proceedings [18] Synthetic anabolic steroids have been in use in clinical medicine since 1940. The Analysis of Steroids in Urine Their analysis become important in 1970s, when methods for their detection were developed as part of doping control programs in athletics. A selected method is provided that allows the detection from most of the anabolic steroids (structurally related to testosterone molecule- ethylestrenol, methyl testosterone, methandienone etc) of interest in athletic doping control 23-Nov-11 33

Astrochemistry [19] :

34 Astrochemistry [19] Several GC-MS have left earth. Two were brought to Mars by the Viking program. Venera 11 and 12 and Pioneer Venus , analyzed the atmosphere of Venus with GC-MS. The Huygens probe of the Cassini-Huygens mission landed one GC-MS on Saturn's largest moon, Titan. The material in the comet Gerasimenko will be analyzed by the Rosetta mission with a GC-MS in 2014. 23-Nov-11 34

Limitations [4]:

35 Limitations [4] Compounds with lower vapor pressures cannot be analyzed. Determining positional substitution on aromatic rings is often difficult. Certain isomeric compounds cannot be distinguished by mass spectrometry (for example, naphthalene versus azulene). MS must be tuned & calibrated before meaning full data can be obtained. Requires computer with large storage system. Expensive than others. Interpretation of result requires highly trained persons


36 23-Nov-11 36 References Willard H., Merritt L., Dean J., Settle F., Instrumental methods of Analysis .7 th Edition, CBS Publisher & Distributors, 1986, New Delhi, 480, 540-544,569-572 J Mendham R.C. Denney J.D. Barnes M Thomas. Vogel’s Textbook of Quantitative Chemical Analysis . 6 th Edition, Pearson Education, 2005, 350 Skoog D., Holler F., Niemen T., Principles of Instrumental Analysis. 5 th Edition, Thomson Books, 2005, 718-720 McMaster M., McMaster C., GC/MS A Practical User’s Guide. 1 st Edition, WILEY-VCH publication,1998, 4-10 Frost R.,Gautier D., Journal Of Analytical Technology. 2006, 30 (3), 210-215 Chatwal G., Anand S., Instrumental Methods of Chemical Analysis. 5 th edition, Himalaya publication house, 2006, 2.691-2.699. 23-Nov-11 36

PowerPoint Presentation:

37 23-Nov-11 37 Ellis L. and Fincannon A, Organic Geochemistry. 1998, 29 (5-7), 1101-1117 Müller A., Düchting P., Weiler E., Planta. 2002, 216(1), 44-56. Min An, Pratley J., Haig T., Rapid Communications in Mass Spectrometry. 1998,10 (1), 104 - 105 http://en.wikipedia.org/wiki/Gas_chromatography-mass_spectrometry (accessed 14/10/2008) . http://www.chemsoc.org/ExemplarChem/entries/2004/westengland_smith/ExempWeb/GC-MS.htm. (accessed14/10/2008) http://en.wikipedia.org/wiki/Gas _chromatography-mass _spectroscopy.” (accessed 14/10/2008) http://www.kcl.ac.uk/ms-facility/gcms.html. (accessed 12/10/2008) http://www.gmu.edu/departments/SRIF/tutorial/gcd/gc-ms2.html. (accessed 12/10/2008) http://www.gmu.edu/departments/SRIF/tutorial/gcd/pc..html (accessed 13/10/2008) 23-Nov-11 37

PowerPoint Presentation:

38 23-Nov-11 38 http://www.science24.com/paper/6544 (accessed 14/10/2008) http://www.ncbi.nlm.nih.gov/pubmed/15733837 (accessed 14/10/2008) http://pubs.acs.org/cgi-bin/abstract.cgi/ancham/1973/45/i06/f-pdf/f_ac60328a006.pdf?sessid=6006l3 (accessed 14/10/2008) http://www.prenhall.com/settle/chapters/ch31.pdf (accessed 14/10/2008) http://www.chem.vt.edu/chem-ed/sep/gc/gc.html. (accessed 14/10/2008) http://www.clu-in.org/download/techdrct/tdmpa_gc- ms_report.pdf. (accessed 14/10/2008) http://fate.clu-in.org/gc.asp?techtypeid=44 (accessed14/10/2008) http://www.chem.vt.edu/chem-ed/ms/ms-intro.html. (accessed 14/10/2008) http://caag.state.ca.us/bfs/toxlab/gcms.html. (accessed 14/10/2008)

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39 23-Nov-11 39 THANK YOU

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