Mass spectrometry

For what purposes MS is used?

 For measuring the molecular mass of a sample.
 For identification of the unknown compounds little as 10-
12
g, 10-15 moles ; compounds identified at very low
concentrations (one part in 1012) in chemically complex
mixtures.
 For quantification of known compounds.
 Used to discover the number of isotopes ,determine the
relative abundance of the isotopes and measure of their
exact masses.
 Within an accuracy of 0.01% of total weight of sample and
within 5 ppm for small organic molecules
 helps to determine the chemical and structural
information about molecules.
 Fragment sample & analyse products.
 Uses a machine called Mass Spectrometer.
 Electron Ionization (EI) technique

EI is the most appropriate technique for relatively small (m.w.<600) neutral organic molecules
which can easily be promoted to the gas phase without decomposition, i.e. volatile. Since EI
samples are thermally desorbed to the gas phase and subjected to the high energy of EI,
analytes must be thermally stable. The gas phase molecules enter into the ion source where
they are bombarded with free electrons emitted from a filament (Figure 1). The electrons
bombard the molecules causing a hard ionization that fragments the molecule, and turn into
positively charged particles called ions.
 X

Cl
Cl DCM/NEt 3 Ru O
Ru Ru
Cl Stirr, 12 h Cl O
Cl
O OH
X
X= H, LH1 X= H, 1
Br, LH2 Br, 2
Ph, LH3 Ph, 3
MALDI | Matrix Assisted LASER Desorption Ionization Technique
It is a soft ionization technique under desorption ionization methods, which
uses pulsed LASER (Light Amplification by stimulated Emission of Radiation)
beam.

It is used to determine the molecular weight of peptides, antibodies, protiein

molecules etc. up to the size of 300 Kda.

Matrix compound α-cyano-4-hydroxycinnamic acid (CHCA), 2,5-

dihydroxybenzoic acid (DHB), 2-(4-hydroxyphenylazo) benzoic acid (THAP),
sinapinic acid (SA) and 2-(4-hydroxy-phenylazo) benzoic acid (HABA).