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EXPERIMENT 6 : THIN LAYER CHROMOTOGRAPHY OF ANALGESIC DRUGS

Objectives

1) Determine the Rf value.


2) To identify the components in the analgesic tablet by a TLC comparison 1with
standard compounds.

Introduction

Chromatographic are used extensively in organic chemistry laboratories for


routines analysis. Thin layer chromotography (TLC) can be used to determine the
purity of compound , to analyze 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 aaplied 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 is are in
solution . In principle , the components will differ in solubility and in the 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 , it will dried and the developing components will be
visualised . UV lamp and iodine are used to visualized the components .

In this experiment the TLC was used to examine the composition of known
analgesic whic is the pain relieving drug such as paracetamol. Several common
analgesics are aspirin and acetomeniphen . Caffein is sometimes added to these
formulations to overcome drowsiness.

The distance travelled by each component is measured and this value is


called the retardation factor which is designated as Rf value.Rf value for a component
is calculated using the following expression :

Rf = Distance traveled by the component

Distance traveled by the solvent


There is some chemicals that we are using in this experiment are shown below.

Acetaminophen

Aspirin

Caffeine
Result and observation

Label A (aspirin) B (upthamol) C (caffeine) D


(acetaminophen)
Reading 1 - 2.6 cm 2.3 cm 1.1 cm 2.5 cm
Distance
travelled from
start line to
center
spot(cm)
Reading 2 - 2.8 cm 2.4 cm 1.1 cm 2.4 cm
Distance
travelled from
start line to
center
spot(cm)

(TLC reading 2) (TLC reading 1)

The distance from starting point to the end point of reading 1 is 5 cm while for
reading 2 is 5.1 cm

Rf = Distance traveled by the component

Distance traveled by the solvent

Calculation for reading 1

Rf of A (aspirin) = 2.6 / 5 = 0.52

Rf of B (upthamol) = 2.3 / 5 = 0.46

Rf of C (caffeine) = 1.1 / 5 = 0.22

Rf of D (acetaminophen) = 2.5 / 5 = 0.5


Calculation for reading 2

Rf of A (aspirin) = 2.8 / 5.1 =0.55

Rf of B (upthamol) = 2.4 / 5.1 = 0.47

Rf of C (caffeine) = 1.1 / 5.1 = 0.22

Rf of D (acetaminophen) = 2.4 / 5.1 = 0.47

The TLC reports that the drug containing is caffeine

Discussion

Thin layer chromotography is a special of adsorption in which thin layer of adsorbent


supported on a flat surfaces is utilized instead of a column of adsorbent , in a simple words
thin layer chromatography techniques is used to separate mixtures.Thin layer
chromotography techniques was performed on a sheet of glass or aluminium foil which is
coated with thin layer adsorbent material usually silica gel.This layer was known as
stationary phase.Silica gel is a form of silicon dioxide , the silicon atoms are joined via
oxygen atoms in a giant covalent structure .However at the surface of the silica gel , the
silicon atoms are attached to hydroxyl group . The surface of the silica gel is very polar , this
is because of the hydroxyl igroup it can formed hydrogen bonds with suitable compounds
around it as well as van der waals dispersion forces and dipole-dipole attraction.

Differrent compounds in the sample mixture travel at different rates due to the
differances in their attraction to the stationary phase and because of differences in solubility
in the solvent . Fom the above calculation we can see that different compound has different
Rf value.

For reading 1 , Rf for aspirin is 0.52 , upthamol is 0.46 , caffein is 0.22 and
acetaminophen is 0.5 . From reading 2 Rf value for aspirin is 0.55 , upthamol is 0.47 , caffein
is 0.22 and acetaminophen is 0.47 . Reading 1 and 2 has same reading Rf value for caffeine
so the drug is caffeine .

There is some precaution that we should be aware by doing this experiment which is
we cannot allow UV light to shine to anyone eyes , it can cause permanent eyes damage
.While we are doing line on the TLC sheet we should use pencil instead of pen because it
can contaminated our TLC paper.The solution point maybe moves with the pen ink.
Conclusion

The Rf value was determined which is for reading 1 ,Rf for aspirin is 0.52 ,
upthamol is 0.46 , caffein is 0.22 and acetaminophen is 0.5 while for reading 2 , Rf value for
aspirin is 0.55 , upthamol is 0.47 , caffein is 0.22 and acetaminophen is 0.47 .From the
calculation the compound in the TLC tablet is caffeine.

References

1) http://www.chemguide.co.uk/analysis/chromatography/thinlayer.html

2)http://www.google.com.my/imgres?q=acetaminophen+structure&hl=en&biw=630&bih=523&tbm
=isch&tbnid=DJB2GqHcyJYSwM:&imgrefurl=http://chemistry.about.com/od/factsstructures/ig/Chem
ical-Structures---A/Acetaminophen---
Paracetamol.htm&docid=fzax4ltjyeRdUM&imgurl=http://0.tqn.com/d/chemistry/1/0/t/M/1/paracet
amol.jpg&w=500&h=242&ei=ue6sUezsG8XPrQeSjoDQCg&zoom=1&ved=1t:3588,r:0,s:0,i:159&iact=r
c&dur=688&page=1&tbnh=146&tbnw=302&start=0&ndsp=7&tx=208&ty=34

3)http://www.google.com.my/imgres?q=aspirin+structure&hl=en&biw=630&bih=523&tbm=isch&tb
nid=r5x16yeF4Rsd6M:&imgrefurl=http://chemistry.about.com/od/factsstructures/ig/Chemical-
Structures---A/Acetylsalicylic-Acid---
Aspirin.htm&docid=WwEehinkioHn4M&imgurl=http://0.tqn.com/d/chemistry/1/0/4/g/1/acetylsalicy
lic_acid.png&w=325&h=396&ei=1u6sUZC1OtCHrAfxyYAw&zoom=1&ved=1t:3588,r:1,s:0,i:159&iact=
rc&dur=3593&page=1&tbnh=212&tbnw=174&start=0&ndsp=8&tx=86&ty=102

4)http://www.google.com.my/imgres?q=caffeine+structure&hl=en&biw=630&bih=523&tbm=isch&t
bnid=S5lQYargb83f1M:&imgrefurl=https://en.wikipedia.org/wiki/Caffeine&docid=a2ncv-
MklN_BLM&imgurl=https://upload.wikimedia.org/wikipedia/commons/thumb/5/5e/Caffeine-2D-
skeletal.svg/200px-Caffeine-2D-skeletal.svg.png&w=200&h=165&ei=8u6sUdrUFcuArgft-
oCwDg&zoom=1&ved=1t:3588,r:1,s:0,i:159&iact=rc&dur=657&page=1&tbnh=132&tbnw=156&start
=0&ndsp=8&tx=118&ty=82

Questions

1) What happens if the spots are made too large when preparing a TLC plate for
development?

If the spot too large it may cause the shape of the final spot become skewed and
elongates.

2) What happens if the spots are made too small when preparing a TLC plate for
development ?

If the spots are too small the Rf value are hard to determined.
3) Why must the spots be above the level of the developing solvent in the
development chamber ?

Because the spot will move upward from the solvent level and carry the components
of the spot at constant rate to the top but if the spot is below the solvent level , then
the sovent will wash away the spot into the solvent and there will no development.

4) What would happen if the spotting line and positions marked on the plate with
a ball-point pen?

This will make the ink of the ball pen will contaminated the result , the ink will move
with the spot and we cannot get the correct result.

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