GC-MS and its applications


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GC-MS and its applications


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SEMINAR On GC-MS & ITS APPLICATIONS Presented by Samadana Prabhu 611235004015 Master Degree In Pharmacy Under the guidance of Dr.J.V.L.N.Seshagiri Rao.,Professor N.K.Sahoo.,Assistant Professor Andhra University


Content Introduction Principle Instrumentation Working Applications Limitations Conclusion References 18/02/2013 Samadana Prabhu 2


Introduction 1 Gas chromatography-Mass spectroscopy (GC-MS) is one of the so-called hyphenated analytical technique As the name implies, it is actually two techniques that are combined to form a single method of analyzing mixtures of chemicals Gas chromatography is a technique capable of separating, detecting and partially characterizing the organic compounds particularly when present in small quantity. Mass spectroscopy provides some definite structural information from in small quantity. 18/02/2013 Samadana Prabhu 3

Cont… :

Cont… Combination of GC-MS provides extremely powerful tool because it permits direct and effectively continuous correlation of chromatographic and mass spectroscopic properties The separation and identification of the components of complex natural and synthetic mixture are achieved more quickly than any other technique with less sample 18/02/2013 Samadana Prabhu 4

Principle of GC-MS2:

Principle of GC-MS 2 The sample solution is injected into the GC inlet where it is vaporized and swept onto a chromatographic column by the carrier gas (usually helium). The sample flows through the column and the compounds comprising the mixture of interest are separated by virtue of their relative interaction with the coating of the column (stationary phase) and the carrier gas (mobile phase ). The latter part of the column passes through a heated transfer line and ends at the entrance to ion source where compounds eluting from the column are converted to ions. 18/02/2013 Samadana Prabhu 5

GC-MS Instrument:

GC-MS Instrument 18/02/2013 Samadana Prabhu 6 The insides of the GC-MS, with the column of the gas chromatograph in the oven on the right.


Instrumentation 18/02/2013 Samadana Prabhu 7


Instrumentation 2 The GC-MS is composed of two major building blocks: the gas chromatograph and the mass spectrometer The gas chromatograph utilizes a capillary column which depends on the column's dimensions (length, diameter, film thickness) as well as the phase properties . The difference in the chemical properties between different molecules in a mixture will separate the molecules as the sample travels the length of the column. The molecules are retained by the column and then elute (come off of) from the column at different time 18/02/2013 Samadana Prabhu 8

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This allows the mass spectrometer downstream to capture, ionize, accelerate, deflect, and detect the ionized molecules separately. The mass spectrometer does this by breaking each molecule into ionized fragments and detecting these fragments using their mass to charge ratio. 18/02/2013 Samadana Prabhu 9

Samples3&4 :

Samples 3&4 State Organic compounds must be in solution for injection into the gas chromatograph. The solvent must be volatile and organic (for example, hexane or dichloromethane). Amount Depending on the ionization method, analytical sensitivities of 1 to 100 pg per component are routine. Preparation Sample preparation can range from simply dissolving some of the sample in a suitable solvent to extensive. Clean up procedures using various forms of liquid chromatography. 18/02/2013 Samadana Prabhu 10

Types of Ionisation5:

Types of Ionisation 5 Electron impact ionisation Chemical Ionisation 18/02/2013 Samadana Prabhu 11

Mass Analyzers6:

Mass Analyzers 6 Single deflection magnetometer Double focussing Ion collector Time of flight system quadrupole 18/02/2013 Samadana Prabhu 12

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Interfacing GC with Spectroscopic Methods 7:

Interfacing GC with Spectroscopic Methods 7 Elutes from column collected as separate fractions after being detected - composition measured by Mass Spectrometry or IR. Limitation - small ( micromolar ) composition of the solute. Procedure still useful for qualitative analysis of multi-component.

Interfacing GC with Spectroscopic Methods:

Interfacing GC with Spectroscopic Methods GC equipment can be directly interfaced with rapid-scan Mass Spectrometers. The flow rate is usually small enough to feed directly into the ionization chamber of the Mass Spectrometer. Packed columns use a jet separator, which removes the carrier gas for the analyte .

Interfacing GC with Spectroscopic Methods:

Interfacing GC with Spectroscopic Methods Increase momentum of heavier analyte molecules so that 50% or more go into the skimmer. Lighter helium molecules are deflected by vacuum and pumped away. Use to identify components present in natural and biological systems. odor/flavor of foods – pollutants.

Jet Separator8&9:

Jet Separator 8&9 Two capillary tubes aligned with a small space between them. (1 mm) A vacuum is created between the two tubes using a rotary pump. The GC effluent enters the vacuum region, those molecules which continue in the same direction enter the second capillary tube and continue to the ion source.

Jet Separator:

Jet Separator The carrier gas molecules are more easily diverted from the linear path by collisions. The analyte molecules are much larger and carry more momentum. The surface of the separator must be inactive and a reasonably even temperature. Prone to leaks.

Jet Separator:

Jet Separator


Analysis A mass spectrometer is typically utilized in one of two ways: Full Scan or Selective Ion Monitoring (SIM). The typical GC/MS instrument is capable of performing both functions either individually or concomitantly, depending on the setup the particular instrument. 18/02/2013 Samadana Prabhu 20

ApplicationS10 :

ApplicationS 10 Environmental monitoring and cleanup Criminal forensics Law enforcement Sports anti-doping analysis Food, beverage and perfume analysis Astro chemistry Pharmaceutical Analysis 18/02/2013 Samadana Prabhu 21

PharmacEutical Analysis :

PharmacEutical Analysis Prostaglandins and Thromboxanes Steroids Carbohydrates Lipids Amino Acids and Peptides Plant Product 18/02/2013 Samadana Prabhu 22

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Environmental Monitoring and Cleanup GC-MS is becoming the tool of choice for tracking organic pollutants in the environment. The cost of GC-MS equipment has decreased significantly, and the reliability has increased at the same time, which has contributed to its increased adoption in environmental studies. There are some compounds for which GC-MS is not sufficiently sensitive, including certain pesticides and herbicides, but for most organic analysis of environmental samples, including many major classes of pesticides, it is very sensitive and effective.

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GC/MS is a technique that can be used to separate volatile organic compounds (VOCs) and pesticides. Portable GC units can be used to detect pollutants in the air, and they are currently used for vapor intrusion investigations. However other uses of GC or MS, combined with other separation and analytical techniques, have been developed for radio nuclides, explosive compounds such as Royal Demolition Explosive (RDX) and Trinitrotoluene (TNT), and metals.

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Criminal Forensics GC-MS can analyze the particles from a human body in order to help link a criminal to a crime. The analysis of fire debris using GC-MS is well established, and there is even an established American Society for Testing Materials (ASTM) standard for fire debris analysis. GCMS/MS is especially useful here as samples often contain very complex matrices and results, used in court, need to be highly accurate .

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Law Enforcement GC-MS is increasingly used for detection of illegal narcotics, and may eventually supplant drug-sniffing dogs. It is also commonly used in forensic toxicology to find drugs and/or poisons in biological specimens of suspects, victims, or the deceased.

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Security A post-September 11 development, explosive detection systems have become a part of all US airports . These systems run on a host of technologies, many of them based on GC-MS. There are only three manufacturers certified by the FAA to provide these systems , one of which is Thermo Detection (formerly Thermedics ), which produces the EGIS, a GC-MS-based line of explosives detectors. The other two manufacturers are Barringer Technologies, now owned by Smith's Detection Systems, and Ion Track Instruments, part of General Electric Infrastructure Security Systems.

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Astrochemistry Several GC-MS have left earth. Two were brought to Mars by the Viking program. Venera 11 and 12 and Pioneer Venus analysed 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 67P/ Churyumov-Gerasimenko will be analysed by the Rosetta mission with a chiral GC-MS in 2014.

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Medicine Dozens of congenital metabolic diseases also known as Inborn error of metabolism are now detectable by newborn screening tests, especially the testing using gas chromatography-mass spectrometry. GC/MS can determine compounds in urine even in minor concentration. These compounds are normally not present but appear in individuals suffering with metabolic disorders. This is an increasingly becoming a common way to diagnose IEM for earlier diagnosis and institution of treatment eventually leading to a better outcome.

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It is now possible to test a newborn for over 100 genetic metabolic disorders by a urine test at birth based on GC/MS. In combination with isotopic labeling of metabolic compounds, the GC-MS is used for determining metabolic activity. Most applications are based on the use of 13 C as the labeling and the measurement of 13 C/ 12 C ratios with an isotope ratio mass spectrometer ( IRMS ); an MS with a detector designed to measure a few. 18/02/2013 Samadana Prabhu 30

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Food, Beverage and Perfume Analysis Foods and beverages contain numerous aromatic compounds, some naturally present in the raw materials and some forming during processing. GC-MS is extensively used for the analysis of these compounds which include esters, fatty acids, alcohols, aldehydes , terpenes etc. It is also used to detect and measure contaminants from spoilage or adulteration which may be harmful and which is often controlled by governmental agencies, for example pesticides. 18/02/2013 Samadana Prabhu 31


LimitationS Only compounds with vapor pressures exceeding about 10–10 torr can be analyzed by gas chromatography-mass spectrometry (GC-MS). Determining positional substitution on aromatic rings is often difficult. Certain isomeric compounds cannot be distinguished by mass spectrometry (for example, naphthalene versus azulene ), but they can often be separated chromatographically. 18/02/2013 Samadana Prabhu 32


conclusion I here by conclude that GC-MS is one of the best analytical tool in analysing the most of the compounds. What makes GC-MS as an analytical method of option is its increased sensitivity and reliability even in very small quantities( ng ) 18/02/2013 Samadana Prabhu 33


References gas chromatography-mass spectroscopy from Wikipedia ,The free encyclopedia. Principles and Intrumentation of gas chromatography-mass spectroscopy by W. M. A. Niessen , hyphen MassSpec Counsultancy,Leiden,The Netherlands. Gas chromatography by U. A. Devkate Sir. Encyclo pedia of Chromatography – Jack Cazes Gas chromatography by Ian A[1]. Fowlis 2 nd Edition hollas_J.M ._ modern _Spectroscopy Handbook of Instrumental Technique for Analytical Chemistry by Frank Settle. Moderm Instrumentation Methods and Techniques by Francis Rouessac and Annick Rouessac . Instrumental methods of Analysis by Willard,Merritt,Dean,Settle,7 th Edition. http:/ wikipedia / applications_of_massspectroscopy /



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