OBJECTIVE

To examine the composition of a known analgesic (pain relieving) drug such as Panadol by
using thin layer chromatography (TLC).

INTRODUCTION

Chromatographic are used extensively in organic chemistry laboratories for routines analysis.
Thin layer chromatography (TLC) can be used to determine the purity of compound, to
analyse the composition of a mixture are differentiated by exposing to two competing phases,
the stationary phase is a polar adsorbent such as silica gel or alumina, which has been coated
on plastic plate. The mobile phase is an organic solvent. The solvent moves up the plate
capillary action.

As the solvent moves past the spot that was applied, an equilibrium was achieved for
each component of the mixture between the molecules of that component which are adsorbed
on the solid and the molecules which are in solution. Theoretically, the components will
differ in solubility and in strength of their adsorption to the adsorbent and some components
will be carried further up the plate than the others. When the solvent has reached on the top of
the plate, the plate will be removed from the solvent, dried and the developing components
will be visualised. UV lamp and iodine are used to visualise the components.

In this experiment, TLC was used to examine he composition of known analgesic

which is the pain relieving drug such as paracetamol. Several common analgesics are aspirin
and acetaminophen. Caffeine is sometimes added to these formulations to overcome
drowsiness.

The distance travelled by each component is measured and the value is called the
retardation factor which is designated as Rf value. Rf value for a component is calculated
using the following expression:
CHEMICALS / REAGENTS

Aspirin, caffeine and acetaminophen as reference materials

An analgesic tablet

0.5% glacial acetic acid in ethyl acetate

Ethanol

Dichloromethane

APPARATUS

Capillary tubes

Silica gel 60 F – 254 chromatographic plates

Development chamber
PROCEDURE

1. At least 5 micropipettes are prepared for sample spotting

2. Samples of aspirin, caffeine, acetaminophen and Panadol are prepared by dissolving
about 10 mg of compound in 1.0 mL of 1:1 methylene chloride/ethanol on a watch glass.
More than 0.1 g of any chemical was not taken. A glass rod is used to crush the pill into
powder. Some of the samples may not fully dissolve, but do not add more solvent (if
desired, the samples are warm using a hot water bath or hot plate). Regardless, there will
be enough chemical dissolved to spot and detect using the UV lamp.
3. Spotting technique on a sheet of filter paper or towelling is practiced until satisfied that
narrow diameter samples can be applied, and pipettes are reliable.
4. A very light pencil line at 1 cm from the bottom of mini TLC plate is drawn (the pencil is
made sure does not gouge out the adsorbent).
5. Samples are spotted on the line in a predetermined order or, even better, the samples are
coded in pencil at the top of the TLC plate. The plate is spotted from left to right
beginning with acetaminophen (Ac), aspirin (As), caffeine (Cf) and Panadol (Pa).
6. The TLC plate is carefully placed into the developing chamber so that the bottom f the
plate is flat in the ethyl acetate developing solvent and the plate does not touch the filer
paper. The developing chamber is closed carefully without disturbing the TLC plate. the
solvent front should be rising along the TLC plate evenly.
7.

RESULTS
DISCUSSION

CONCLUSION
QUESTION
REFERENCES