LAQ 3003 Analytical Chemistry Ш
Assignment 2
Gas Chromatography- Mass Spectrometry (GCMS)
Submitted to: Prof. Gisselle Norville Submitted by: Analytes
Prepared by Student ID Email address
Manveer Kaur C0894571
[email protected] Mandeep Kaur C0887205
[email protected] Manpuneet Kaur C0887189
[email protected] Veerpal Kaur C0894570
[email protected] Neha Chaudhary C0894562
[email protected] Introduction: Gas chromatography–mass spectrometry (GC–MS) is a technique that blends the
capabilities of gas chromatography and mass spectrometry to analyze and identify various
substances in a sample. GC-MS has been a go-to method for analyzing biological samples for
many years. It's widely used by the US National Institute of Standards and Technology and other
organizations to develop precise methods for validating standard reference materials. This
technique is essential for accurately measuring concentrations of various clinically important
substances like cholesterol, glucose, steroid hormones, creatinine, and urea nitrogen in reference
materials.
Gas chromatography (GC) is a technique used to separate and detect the components of a
sample, providing information about their presence and quantity. However, GC alone offers
limited data, typically just retention times and detector responses, which are compared to known
standards for identification. To identify unknown substances more effectively, GC is often paired
with mass spectrometry (MS). This combination enhances the analysis by allowing more detailed
detection and identification, with MS serving either as the primary detector or working alongside
GC detectors.
Principle of operation: The principle of operation for GC-MS involves two main stages: gas
chromatography (GC) and mass spectrometry (MS).
GC-MS operates by first separating the components of a sample through gas
chromatography, where the sample is vaporized and carried by an inert gas through a
column.
The different compounds in the sample separate based on their interactions with the
stationary phase and their volatilities, resulting in distinct retention times.
These separated compounds are then introduced into a mass spectrometer, where they are
ionized and broken into charged fragments.
These fragments are analyzed based on their mass-to-charge ratio, producing a mass
spectrum that helps identify the compounds. This combination of separation and
identification allows GC-MS to analyze and identify complex mixtures effectively.
Parts of GCMS:
Sample Injector: Sample is injected into the system and vaporized before entering the
column.
Carrier Gas Supply: Inert gas (e.g., helium, nitrogen) is used to transport the sample
through the column.
Chromatographic Column: A narrow tube packed with a stationary phase material where
the separation of sample components occurs.
Oven: Used to control the temperature, influencing the separation process.
GC Detector: Detects the separated compounds as they elute from the column, producing a
chromatogram.
Ion Source: The compounds exiting in the GC are ionized here using electron impact to
create charged fragments.
Mass Analyzer: A magnetic or electric field is used to separate the ionized fragments based
on their mass-to-charge ratio (m/z)
MS Detector: Records the abundance of the separated ions, generating a mass spectrum.
Data System: Collects and processes the data from the GC and MS, allowing for the
interpretation and identification of the sample components.
GC-MS Procedure Overview
Sample Injection: The sample is introduced into the gas chromatograph (GC), either
manually or by an autosampler. In liquid samples, the liquid is vaporized in the heated GC
inlet and then transported through the column.
Separation: The sample components (analytes) are separated based on their interaction with
the stationary phase in the chromatographic column, which is usually a liquid phase in a
narrow, short column.
Transfer to Mass Spectrometer: After separation, the neutral molecules exit the GC
column and are carried through a heated transfer line into the mass spectrometer.
Ionization: In the mass spectrometer, the molecules are ionized, typically by electron
ionization (EI). An electron impacts the molecules, creating a molecular ion and resulting in
fragment ions due to bond breakage and rearrangements.
Mass Analysis:The ions are separated based on their mass-to-charge ratio (m/z) using a mass
analyzer. Various types of mass analyzers are used, such as:
o Quadrupole: Scans ions by varying voltage, allowing only ions of specific m/z values to reach
the detector. Operates in full scan mode or selected ion monitoring (SIM) mode.
o Ion Trap: Traps ions in three-dimensional orbits and ejects them sequentially.
o Time-of-Flight (ToF): Separates ions based on their time of flight through a tube; faster for
lighter ions and slower for heavier ones.
o Magnetic Sector: Uses electric and magnetic fields to bend ion trajectories for separation.
o Orbitrap: Ions orbit around a central spindle, with their frequency of movement being m/z-
dependent.
Detection and Data Analysis: Ions are detected by an electron multiplier or a multi-channel
plate, depending on the resolution of the mass spectrometer. The detected signals are
recorded by acquisition software, producing a chromatogram and a mass spectrum for data
interpretation.
Applications of GCMS:
Environmental Analysis: Detects and quantifies pollutants, pesticides, and other
contaminants in air, water, and soil samples.
Clinical Diagnostics: Analyzes biomarkers, drugs, and metabolites in biological fluids for
diagnostic purposes.
Pharmaceuticals: Used in drug development and quality control to identify and quantify
drugs and their metabolites.
Forensic Science: Identifies substances in crime scene evidence, such as drugs, explosives,
and poisons.
Food and Beverage Industry: Assesses flavor compounds, additives, and contaminants in
food products.
References:
Turner, D. (2022, June 10). GC-MS Principle, Instrument and Analyses and GC-MS/MS.
Analysis & Separations from Technology Networks.
https://www.technologynetworks.com/analysis/articles/gc-ms-principle-instrument-and-analyses-
and-gc-msms-362513
Gross, Jürgen H. Chapter 14 Hyphenated Methods P.831 Mass Spectrometry.
