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of
Coldeze
Super
pharmaceutical cold and flu
remedy solution.
Introduction
Medications intended to treat the common cold often contain a number of active
ingredients which may be separated by various means and analysed. Modern
separation techniques may yield a tranche of both quantitative and qualitative
data regarding the composition of a sample.
An umbrella term for modern separation techniques is chromatography, which
covers a wide range of separatory methods, some of the more widely used
including thin layer chromatography (TLC); gas chromatography (GC), and
reverse phase high performance liquid chromatography (RP - HPLC). Each
approach varies in terms of speed, expense, performance parameters, and so on;
from the more basic information provided by TLC (key data : the Rf = distance
spot
travels
/
distance
solvent
travels)
to
the
multitude
of
quantitative/qualitative/performance parameters which it is possible to
determine via RP-HPLC, for example.
In this procedure, the composition of an oral solution for cold and flu - Coldeze
Super, was investigated and an attempt was made to analyse the exact
proportions of its active ingredients. The stated proportions of the active
substances were 250 mg/5ml paracetamol, 20 mg/ml caffeine and 10 v/v %
ethanol.
detector was utilized, with the method of internal standards for calibration.
(Waters Alliance 2695 System 28, Column: Zebron Waxplus, Column Length
15 metres, Carrier gas hydrogen 5.5psi Flow Rate - ~3ml/min, Injection Temp
100C Injection Temp 230 C Detector 1: 150).
Ethanol
/cm3
1
2
3
4
5
6
7
8
9
10
0.25
0.50
0.75
1.00
1.25
1.50
1.75
2.00
2.25
2.50
Gives %
(v/v)
Ethanol
1
2
3
4
5
6
7
8
9
10
Propan1-ol
/
cm3
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
1.50
Gives %
(v/v)
Propanol
6
6
6
6
6
6
6
6
6
6
A malfunction with the GLC apparatus arose approximately halfway through the
laboratory session, which prevented any further data from being collected. As an
exercise in gaining familiarisation with the techniques involved, data from a
previous session were used in order to plot absolute peak area and peak area
ratios for ethanol and propan-1-ol. (Table 2)
Peak
area
ratio
Peak
area
ratio 2
0.65
0.67627
9
EtOH
27270.5
area 3
3
(V.s)
EtOH
area
mean
26220.2
9
EtOH
area SD
2385.98
8
Peak
area
ratio 3
Peak
area
ratio
mean
Peak
area
ratio SD
0.65302
5
0.66
0.01372
7
Paraceta
mol
concentra
tion
(mg.dm-3)
500
100
50
400
300
200
Paraceta Caffeine
mol area concentra
(V.s)
tion
(mg.dm-3)
Caffeine
area (V.s)
9622455.
1
122868.6
9
1693137.
09
690865.4
9
3937017.
1
2183863.
11
1544197.
36
500
2762202.4
100
526923.5
400
1740623.09
50
3606631.71
200
1185123.68
300
1295327.94
A rough calibration plot was plotted from the data. Due to time constraints it was
not possible to run a duplicate calibration chromatogram.
Next, 2.5cm3 of the unknown oral solution was diluted to 50 cm 3 with methanol,
labelled, then from this, 5 cm3 was taken and diluted to 50cm -3 with methanol.
This was injected and a chromatogram was obtained.
Solve
nt
front
95:5
100
50:5
0
5
5
5
Parac
etam
ol
front
(cm)
2.8
0.7
Parace
tamol
Rf
value
Caffeine
front
(cm)
Caffein
e
Rf
value
Ibuprofen
front (cm)
Ibuprofe
n
Rf
value
Unkno
wn
front 1
Unknow
n f. 1
value
Unkn
own
front
2
U2 Rf value
1.79
7.14
0.85
0.3
5.88
16.6
4.4
3.8
1.14
1.32
0.9
0.25
5.6
20
2.7
0.7
1.85
7.14
method, great care must be taken to ensure accuracy. The data used in this
investigation were of dubious accuracy.
EtOH in unknown =
23489.34; 29275.53, 23489.34
Mean area EtOH in unknown = 24751.40
SD = 2185.95
Calculation of unknown: y = mx + c
y = 4267.6x 5593.2
(y+5593.2) / 4267.6 = x
x = 7.11
Errors appear
to have been
introduced
during
the
procedure of
calibration.
This
was
noted during
the laboratory
session
but
time
constraints
restricted the
availability of
the
HPLC
apparatus. In future the researchers will need to plan more proactively rather
than relying on scheduled as/when availability of equipment.
References
Higson. Seamus. Analytical Chemistry