GAS CHROMATOGRAPHY-MASS

SPECTROMETRY

BY

B.SWATHI
M.Pharm, (1st sem)
SEMINAR IN ANALYSYS
TALLA PADMAVATHI COLLEGE OF
PHARMACEUTICAL SCIENCES
ORUS, KAREEMABAD, WARANGAL.
 INTRODUCTION
GC-MS COMBINATION
GC = Separation

MS = identification

GC can separate volatile and semivolatile compounds

with greater resolution, but it cannot identify them.

MS can provide structural information on most

compounds such that they can be exactly identified,
but it cannot readily separate them.

When GC is combined with MS, a powerful analytical

tool is created.

The symbiotic relationship of these two methods

makes an interesting study in the development of
analytical instruments, as first of a growing class of
“hyphenated” technique.
HISTORY
The use of mass spectrometer as the detector in the gas
chromatography was developed during 1950’s by Roland
Gohlke and Fred McLafferty.

PRINCIPLE
The GC works on the principle that a mixture will separate into
individual compounds when heated.

Sample introduced into GC inlet vapourized at 250 c, swept

onto the He carrier gas and separated on column.

Sample components emerge from column, flowing into the

capillary column interface connecting the GC column and the
MS(He removed).

The computer drives the MS, records the data, and convert the
electrical signals into visual displays and hard copy displays.

Identification of compound based on it’s mass spectrum relies

on the fact that every compound has a unique fragmentation
pattern.

GC/MS can handle mixtures.

The GC portion of GC/MS provides the high resolution of

volatile organic solutes in a mixture in the gas phase.

As each solutes exits the gas column, it is diverted into a mass

spectrometer which is capable of both monitoring the amount
of and identifying the chemical nature of the solute.

Both qualitative and quantitative information about the

mixture can be obtained.
INSTRUMENTATION OF GC-MS
Desired characters:
To be suitable for GC analysis, a compound must have
sufficient volatility and thermal stability. (all or some
compound molecules in the gas or vapour phase at 250 to
350 c or below donot decompose at these temperatures.

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 cleanup
procedures using various forms of liquid chromatography.

Analysis time:
In addition to sample preparation time, the instrumental
analysis time usually is fixed by the duration of the gas
chromatography run, typically between 20 and 100 min. Data
analysis can take another 1 to 20 hr depending on the level of
detail necessary.
GC & MS SCHEMATIC
DIAGRAM:

Injection port: 1 microlitre of solvent containing the

mixture of molecules injected into the GC and the
sample is carried by inert gas through the instrument,
usually helium. The inject port is heated to 300 c to
cause the chemicals to become gases.

Oven: The outer part of the oven is very specialized

oven. The column is heated to move the molecules
through the column, Typical oven temperatures range
from 40 c to 320 c.

Column: Inside the oven is the column which is a 30

meter thin tube with a special polymer coating on the
inside. Chemical mixtures are separated based on their
votality and are carried through the column by Helium.
Chemicals with high votality travel through the column
more quickly than chemicals with low votality.
Ion source: After passing through the GC, the chemical pluses continues
to the MS. The molecules are blasted with electrons, which cause them
break into pieces and turn into positively charged particles called ions.
This is important because ions are to be charged inorder to pass
through the filter.

Filter: As the ions pass through the MS, they travel through an
electromagnetic field that filters the ions based on mass. The filter
continuously scans through the range of masses as the stream of ions
come from the ion source.

Detector: A detector counts the no. of ions with a specific mass. This
information is sent to a computer and a mass spectrum is created. The
mass spectrum is a graph of the no. of ions with different masses that
travel through the filter.
GC MS INTERFACES:
Incompatability of GC & MS

GC operates at atmospheric pressure and MS ion source at 10-5 torr.

10 8 fold pressure difference.

Need of the interface.

Transports the effluent from the gas chromatograph to mass

spectrometer.

Analyte must not condense in the 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.
Types of Mass Spectrometer Detectors

The most common type of mass spectrometer (MS) associated with a gas chromatograph (GC)
is the quadrupole mass spectrometer, sometimes referred to by the Hewlett-Packard (now
Agilent) trade name "Mass Selective Detector" (MSD). Another relatively common detector is
the ion trap mass spectrometer. Additionally one may find a magnetic sector mass
spectrometer, however these particular instruments are expensive and bulky and not typically
found in high-throughput service laboratories. Other detectors may be encountered such as
time of flight (TOF), tandem quadrupoles (MS-MS) (see below), or in the case of an ion trap MS n
where n indicates the number mass spectrometry stages.