HCl in pharmaceutical formulations by kinetic spectrophotometric

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National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
Determination of ranitidine - HCl in pharmaceutical
formulations by kinetic spectrophotometric and flow injection activated chemiluminescence methods .
Abdul Majeed K . Ahamed , Ali I . Khaleel and Suham T. Amine
Chemistry Department, College of Education, Tikrit University.
(
(Received on
3/1 /2006)
NJC)
(Accepted for publication on 15/11/2006)
Abstract
This study involves development of
a simple kinetic
spectrophotometric
method and a new flow injection-activated chemiluminescence (FIA-CL) for the
determination of ranitidine -HCl (R-HCl) in pharmaceutical preparations.
Spectrophotometric method was based on the oxidation of the R-HCl with alkaline
potassium permanganate , the reaction is followed spectrometrically by measuring
the rate of change of the absorbance at 600 nm. A fixed-time (at 30min) method is
adopted for determining the drug concentration . The calibration graph was linear in
the range of (1 - 7) μg-ml-1 with a correlation coefficient of 0.9981,detection limit of
0.183 μg-ml-1 and a relative standard deviation RSD% of 0.58-1.62%.
The method of FIA-CL was based on the activation of luminol-cobalt-H2O2
chemiluminescence by R-HCl. The linearity is (1-6) μg-ml-1 with detection limit of
(0.75) μg-ml-1 , and
correlation
coefficient was 0.9996 (n=6) and the relative
standard deviation was (0.74-1.00)% .
The two methods were applied successfully to determine the content of
R-HCl in pharmaceutical preparations with a recovery of 97-99 % .
‫الخالصة‬
‫تضممم ه همملد الد ارلممة ئلممأ ج مين ن ضلال م ن أل ضممط الجمميء اطوف تطمموير طريقممة طيديممة لتقممد ر دواء ار تممد ن‬
‫ ) و متابعممة التدائ م‬KMnO4 ‫ه دروكلو ار ممد تلممت د ئلممأ ضكلممدد همملا الممدواء مممع سرم مماه السوتال م وط القائديممة‬
‫ مما وم تر ج وجممد ضن المميمن الممسيط لتماميممة‬600 ‫ئ ممد طمموف ممموج‬
‫طيديمما مممن ممسف ليمماب الت ممر باومتممما‬
‫ أل وحد‬0.9981 ‫ م ومعام اورتباط‬/ ‫ ) مايكرو غراط‬11 ‫ م‬1 ‫ دليقة ومدى ال طية تراوح س ن‬30 ‫التدائ هو‬
534
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫ م‬0.58 ‫ تتم مراوح سم م ن‬RSD% ‫القيالم م ال ل ممس‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
‫ مم م ول مميط او حم م ار‬/ ‫ م ممايكرو غم مراط‬0.183 ‫الكش ممد مقم ممدارد‬
‫ ج‬%)1.62
‫ضممما الطريقممة الةا يممة الممت ده ئلممأ تحد ممي السريممظ الكيميممان ل بمماط لوم مموف م س روكل م د ال ممدروج ن م‬
‫ م م‬/ ‫ ) مممايكرو غ مراط‬10.0 ‫ م‬1.0 ‫كوبلممه ) سوالممطة همملا الممدواء وكا ممه الحممدود ال طيممة للطريقممة تتممرواح س م ن‬
) 0.75 ‫ وحممد كشم ممد‬%1.00 ‫ م‬%0.74 ‫ت مراوح س م ن‬
‫لممس منممو‬
‫ليال م‬
‫ وا ح م ار‬0.9996 ‫وبمعام م ضرتبمماط‬
‫ م ج‬/ ‫مايكرو غراط‬
‫ ج‬%) 99 ‫م‬97
‫طبقه هات ن الطريقت ن س جاح ئلأ الملتحضراه الم دو ية وكان اولترداد المنو‬
Introduction
or pale yellow , crystalline powder ,
Ranitidine(1)- HCl ( R - HCl ):
freely soluble in water and methanol .
The empirical formula for R-HCl is
N,N - Dim ethyl – 5 – [ 2 ( 1- methyl
C13H22N4O3S.HCl and its molecular
amino - 2 - nitro vinyl amino ) ethyl
weight is 350.9 , it is used as(2) inhibits
thio methyl ] furfuryl amine is a white
gastric acid secretion and its structure
is:
O
Me2N
H
NO2
N
.
S
This drug
HCl
NHMe
has been determined in
The present paper describes a
tablets and ampoules by coluometric(3)
spectrophotometric
and potentiometric(4)
determination
titrations .
method for the
of
(R-HCl
)in
HPTLC(5,6) and HPLC have been used
pharmaceutical preparations based on
for the determination of R-HCl using
the oxidation with alkaline potassium
C18
permanganate. This study also includes
column
at
different
mobile
phases(7-9) .
development of FIA-CL method
De Almeida(10) and chattoraj(11) used
Experimental
UV/Visible spectrophotometry for the
A) spectrophotometer apparatus for
determination of (R-HCl)in tablets
pharmaceutical
preparation,
determination the absorbance,
the
the spectrophotometer used was
absorbance was measured at 314nm
Philips
with linearity ranged from 2-30 g/ml.
535
model
pu
8720
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
uv/visible, with quartus cells of
powder in 1L of (0.7μg.ml-1) cobalt
1 cm width.
(II) solution . Solutions of lower
B)
FIA
Chemiluminescence
concentrations
apparatus
The
were
prepared
by
appropriate dilution .
FIA-CL configuration
is
Pharmaceutical preparation
outlined in figure 1 showing the
Rantism tablets : provided from (
system of chemical reaction used for
SDI ) Samara - Iraq .
the determination of (R-HCl).
Ten tablets were grinded well and a
Reagents
certain portion of the final fine
Reagents of analytical grade and
distilled water were used
powder was accurately weighed to
through
give an equivalent to 150 mg of
o
were
ranitidine – HCl and then dissolved
prepared by appropriate dissolution
with (25ml) of Methanol . The
as shown in table 1.
resulting solution was washing by
out
the
study
Luminol
was
Solutions
prepared
by
shaking with methanol and filtered on
dissolving in a solution of (0.1 M
Whatman filter paper No.4 to remove
Na2CO3) where as
KMnO4
any suspended particles . The filterate
was prepared and standardized with
and washing were evaporated to
0.1M Na2C2O4.
dryness at 60C and the residue was
Hydrogen peroxide solution (1M)
redissolved in distilled water forming
was prepared by diluting 45.72ml of
a
H2O2 (48%) in 1 L of distilled water
concentration .
and standardized against standard 0.1
The same method was adopted for
M KMnO4 .
preparation of Zantac tablets, and the
of
100
of distilled
cobalt
and
ultrasonication
water and standardized against 0.1 M
needed.
Na2CO3 . Cobalt (100μg.ml-1) was
General procedure for the
prepared by dissolving 0.4039 gm of
spectrophotometric method.
CoCl2.6H2O with 20 ml of 5 x10-3 M
H2SO4
and
diluted to 1L
μg.ml-1
final dissolution was in (0.7 μg. ml-1)
0.55 ml of sulfuric acid (96%)
was diluted in 100 ml
solution
was
Initial rate method : Aliquots of
with
0.01M KMnO4 solution ( 1.0ml ) and
distilled water. Finally , R-HCl stock
1.00M NaOH solution ( 2.0 ml ) were
solution (100μg.ml-1) was prepared
transferred into a 10ml volumetric
by
flask. An accurate volume of the
dissolving 0.01 gm of
R-HCl
536
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
working solution of R- HCl (0.1 - 1.2)
the reaction product were optimised
ml was added and diluted to volume
as follows :
with distilled water. The contents of
Effect of the KMnO4 concentration
the mixture were shaken well and
immediately
transferred
spectrophotometric
cell
to
at
To study the effect of the
the
KMnO4 concentration , aliquots of R-
room
HCl containing 100μg .ml-1 were
temperature. The absorbance was
transferred into a series of 10ml
recorded at 600nm as a function of
volumetric
time against reagent blank.
flasks,
followed
by
addition of varying volumes of 0.01M
In the second procedure, the
KMnO4 ( 0.1-1.1 ) ml and 2.0 ml of
absorbance was measured at a fixed
1.00M
time of (30min.) and was plotted
NaOH
solution
.
The
absorbance at 600nm was measured
against the final concentration of R-
at a fixed time of 30 minutes . It is
HCl and the content of the drug was
apparent from figure 2 that the
calculated from either the calibration
absorbance increased with increasing
graph or regression equation .
volume of the KMnO4 solution, and
Results and Discussion
became constant at 0.9ml and so then
Part(1 ) : Kinetic spectrophotometric
1.0ml of KMnO4 was used as the
determination
optimal volume .
of
R-
HCl
in
pharmaceutical preparation .
Effect of the NaOH concentration
The influence of the NaOH
In an alkaline medium , potassium
permanganate oxidizes R-HCl ,
concentration on the formation of
resulting in the formation of
MnO42- was examined critically.
manganate ion(13) , which showed an
Figure3 shows that the maximum
absorption peak at 600nm.
absorbance was obtained with 1.8ml
of the 1.00M NaOH, so the optimum
Because the intensity of the color
increased with time , a kinetically
volume of 2.0ml was chosen.
based method was elaborated for the
Effect of oxidation time
determination of R-HCl in dosage
It was found that the most
forms . Initial parameters for this
acceptable value was obtained at a
study are given in table 2 .
fixed time of 30min., and therefore
The
various
experimental
was considered to be the most
parameters affecting the formation of
537
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
suitable
time
interval
for
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
KMnO4 solution in an alkaline
measurements .
medium of 1M NaOH .
The Ranitidine-HCl contains thio
Final absorbance spectrum of
Ranitidine – HCl
ether linkage which has an ability to
A clear peak of MnO42- at 600nm
be oxidized to the corresponding
( fig.5 ) was obtained after the
sulfoxide(13) . The reaction
oxidation of R-HCl by 0.01M
mechanism is proposed and given in
the following equations .
NO2
H
CH3
O
2
N
S
CH3
+ 2MnO4- + 2 OHNHCH3
CH3
NO2
O
O
2
C
N
H
N
S
C
N
+ 2MnO4-2 + H2O
CH3
NHCH3
Recommended Analytical
concentration range of 1.0- 7μg .ml-1
conditions
with correlation coefficient of 0.9981
and molar absorbance max 2.3 x 104
According to the results obtained ,
L.mol-1 .cm-1 .
the optimum conditions for the
determination of ranitidine-HCl using
The relative standard deviation of
a kinetic spectrophotometric method
the method was 1.62 based on 6
are given in table 3 .
replicate determinations. Table 4
shows summary of analytical data for
Calibration graph
the determination of ranitidine -HCl
A linear calibration graph for
using spectrophotometric method .
ranitidine -HCl ( Fig.6 ) under the
optimized conditions was obtained .
Beers
law
is
obeyed
over
the
538
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
The effect of luminol concentration
Pharmaceutical application
The proposed method was applied
on the net chemiluminescence intensity
for the determination of ranitidine -
was studied . Different concentrations
HCl in tablets . Good precision and
of luminol (1×10-3 –1×10-5 M) are used
recovery were obtained . The method
to establish the best emission intensity
was successfully compared with the
– time profile that can be obtained.
British
Figure 7 shows that (5 × 10-4 M) of
pharmacopoeia
standard
method . The results obtained are
luminol is the optimal concentration .
summarized in table 5 .
The effect of H2O2 concentration
was investigated ; from the results of
figure (8), the concentration of ( 1×10-2
M) H2O2 was selected to be the
optimum concentration .
Part (2) : Determination of ranitidine
-HCl using a new FIA-CL method.
General procedure
Effect of Sulphuric acid and Cobalt
The FIA-CL scheme is outlined in
Concentrations
Figure1. Varying concentrations of RThe effect of the acidity of cobalt
HCl were prepared in Co2+ ( 0.7mg.ml) solution . 150ml aliquot of each
Co2+ solution was also studied ; three
solution was injected through the
concentration of cobalt Co2+ (0.2 , 0.5
sample loop into the stream of Co2+
, 0.7 ) μg . ml-1 with varing
solution , which then was combined
concentrations of (1 × 10-3 - 10 × 10-3 )
with luminol and hydrogen peroxide
M of H2SO4 were investigated . The
streams in the flow cell which situated
best intensity was obtained at the
in front of the photomultiplier tube
concentration
(PMT) .
H2SO4(fig.9).
Results and discussion
The effect of cobalt concentration was
1
The
chemiluminescence
luminol–hydrogen
peroxide–Co
of
(5x10-3)M
of
of
also studied, figure (10) shows that the
(II)
suitable concentration of Co+2 is 0.7 μg
/ ml-1
System is very intense(14). However, in
this work, trace amounts or R-HCl
It is worth noting here that as the
were found to be strongly activate
concentration of H2SO4 increases the
chemiluminescence
CL intensity increases , this is because
signal
of
this
system .
of increasing the catalysed oxidation of
Effect of reagents concentration
luminol by H2O2
(16)
. At 1x10-2 M
H2SO4 the CL intensity decreases , this
539
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
can be attributed to the cleavage of the
analytical data obtained from the
formed fluorescent compound .
calibration graph are summarized in
Table
6
shows
that
as
the
table 9 .
concentration of H2SO4 increases the
time
of
analysis
Interferences
decreases
Ranitidine
-
HCl
is
usually
accompanied with decreasing band
formulated in tablets , and injections
width .
forms , therefore, the effect of some
Effect of flow rate
common excipient substances usually
A flow rate ranged from (1-10)
present in pharmaceutical preparation
ml/ min was investigated . Table 7
were investigated . The presence of
shows that the CL intensity increased
1μg.ml-1 of Aerosil , and 2 μg.ml-1 of
with the increase of flow rate .
Mg-stearale
However , a flow rate of 3ml/min is
interfering
recommended for all streams because
chemiluminescence intensity of 5.0
of satisfactory CL intensity , less
μg.ml-1 of ranitidine -HCl .
gave
no
effect
significant
on
the
Application of developed new FIA-
reagent consumption and short analysis
time .
CL method for the determination of
Recommended Analytical
R-HCl in pharmaceutical
Conditions
preparations
Two types of tablets containing R-
A Summary of the optimum
experimental
conditions
determination
of
for
the
R-HCl
in
HCl were analysed using the
developed method and the results were
pharmaceutical preparations is on table
compared with the British
8.
pharmacopoeia standard method ,
Calibration graph
Table 10 .
A calibration graph of relative
Comparison between the two
chemiluminescence intensity against
methods
the ranitidine -HCl concentration was
The two proposed methods were
established by applying the optimal
compared with other methods as
conditions . The regression equation is
shown in table (11). The value (0.55)
(Y = 7.7714 X + 0.1333 ) , and the
of calculated F for FlA-CL /
linearity is in the range of (1.0 – 6 ) μg
spectrophotometric methods is much
. ml-1 of
R-HCl ( fig. 11 ).The
540
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
less than the value ( 4.95) for tabulated
0.183 μg.ml-1 and RSD% of 1.62%
F which indicates good agreement .
with 99.0 % recovery .
In part (2) the chemiluminescence was
Conclusion
In
part
(1)
a
simple
spectrophotometric
found to be activated by R-HCl and
kinetic
method
this is the base of the developed
was
developed for the determination of
new
ranitidine- HCl in pharmaceutical
method
preparation by oxidation of the R-
simplicity
HCl with alkaline KMnO4 . The
sensitivity
results show good precision and
consumption . The linearity of this
accuracy for the determination of
method
R-HCl in the range of (1-7) μg.ml-1
correlation coefficient of 0.9996
and
(n=6) and RSD% was 1.00% with
correlation
coefficient
of
method
offers
,
The
proposed
advantages
rapidity
and
is
detection
0.9981 with detection limit of
.
low
(1-6)
limit
,
μg
of
high
reagent
.ml-1
,
0.75μg.ml-1and
recovery (98%) .
Table (1) preparation of some solutions
Substance
NaOH
NaCO3
Na2C2O4
KMnO4
Luminol
Molar
Concentration (M)
Dissolved weight (gm)
Final Volume
(ml)
1.0
4.000
100
0.1
0.1
0.1
1 x10-3
10.599
13.390
15.800
0.1772
1000
1000
1000
1000
Table (2) : Initial Experimental parameters for the spectrophotometric method .
Item
1
2
3
4
5
6
Preliminary parameter
Conc . of KMnO4
Conc . of NaOH
Volume of KMnO4
Volume of NaOH
Reaction Time
Wave Length λmax (nm)
541
Value
0.01 M
1.00 M
1.0 ml
2.0 ml
6 min
600 nm
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
Table (3): Optimum conditions for the detrmination of Ranitidine –HCl using
the spectrophotometric method.
No.
1.
Parameter
Value
Conc. Of KMnO4
0.01M
Conc.of NaOH
Fixed time
Vol . of KMnO4
Vol. of NaOH
Temperature
1.00 M
2.
3.
4.
5.
6.
30min
1.0ml
2.0 ml
25Cْ
Table (4) : Analytical data for the determination of R-HCl by the
spectrophotometric method.
Analytical data
Linear range
Correlation coefficient
Value
1.0-7 μg. ml-1
0.9981
Regression equation
Y=0.0461x +0.7324
1.62 %
0.183 μg. ml-1
2.3 x104 L.mol-1.Cm-1
RSD %
Detection limit
εmax
Table (5) : Application of the proposed Spectrophotometric method for the
determination of Ranitidine – HCl in Pharmaceutical Preparations .
Recovery %
Sample
RSD %
Proposed method *
Standard method
Pure R-HCl
99.6
Rantism Tablets
97.8
Zantac Tablets
98.4
 Each result is the average of three determinations .
99.5
97.3
98.6
1.63
1.62
1.60
Table ( 6 ) Effect of sulphuric acid concentration on band width and time of
analysis .
H2SO4 Concentration (M)
1x10-4
5x10-4
1x10-3
5x10-3
1x10-2
Base band width
(mm)
26.0
22.0
16.0
10.0
8.5
542
Time of analysis (sec)
75.0
67.0
55.0
45.0
43.0
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
Table (7) Effect of flow rate on the emission intensity , analysis time and
peak width using 0.7 μg. ml-1 of Co+2.
Flow rate
ml/min
1.0
2.0
3.0
4.0
5.0
6.0
7.0
8.0
9.0
10.0
Intensity (mv)
Analysis time (Sec)
Peak width mm
228
300
500
610
700
790
850
900
910
925
85
55
45
40
35
30
26
20
15
12
27
18
10
8
7
6
5
4
3.5
3.0
Table (8) The recommended analytical conditions for the determination of
Ranitidine –HCl using FIA – Chemiluminescence system.
Parameter
Conc. Of luminal
Conc. Of H2O2
Conc. Of Co+2
Conc. Of H2SO4
Flow rate
Volume of Co+2 injected
Recommended value
5x10-4 M
1x10-2 M
0.7 μg. ml-1
5x10-3 M
3 ml/ min
150 μl
Table (9) Analytical data for the determination of Ranitidine –HCl using FIACL method.
Analytical data
Linear range
Correlation coefficient
Regression equation
RSD %
Average Recovery
Detection limit (D.L)
Value
1.0-6 μg. ml-1
0.9996
Y = 7.7714 X + 0.1333
1.0%
99.0 %
0.75 μg. ml-1
543
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
Table (10) Application of the proposed method for the determination of
Ranitidine –HCl in pharmaceutical preparations
Sample
Pure Ranitidine-HCl
Rantism Tablets
Zantac Tablets
Recovery %
Proposed method
Standard method
99.0
99.3
98.65
99.2
98.30
99.12
RSD %
1.76
1.72
1.69
Table (11) The statistical comparison of results for the spectrophotometric and
FIA-CL method with other methods
Regression
equation
The method
Y=0.0461
X+0.7321
Y= 7.7714
X+0.1333
_____
_____
_____
_____
spectrophotometric
FIA-CL
HPLC
HPTLC
Coulometric titration
Polarography
Linearity
(μ g/ml)
Correlation
Coefficient
(r)
Recovery
%
RSD
%
ttable
Ref
.
1.0-7.0
0.9981
97-98
1.62
32.72
___
1.0-6.0
0.9996
98-99
1.00
63.26
___
1.5-20
5.0-10
5.0-9.0
3.5-15
0.9978
0.9969
_____
0.9970
93.00
94.50
92.70
98.00
4.50
5.45
1.40
2.30
_____
_____
_____
_____
5
8
3
31
P
Water a
H 2O 2 b
Luminol
V
f
d
R
c
W
Fig (1): Chemical reaction manifold used for the Flow-Injection
Chemiluminescence determination of Ranitidine-HCl.
P- Peristaltic pump V- Injection valve
Photomultiplier
R- Recorder W- Waste solution .
544
F- Flow cell
d-
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
0,4
0,3
e
Absorbance
0,35
0,25
0,2
0,15
0,1
0,05
0
0
0,2
0,4
1
0,8
0,6
1,2
Volume of KMnO4(ml)
Fig (2) : Effect of the volume of 0.01M KMnO4 on the intensity of color
produced for the reaction (Ranitidine-HCl 10μg / ml , 2.0 ml of 1 M
NaOH)
0,5
0,45
Absorbance
0,4
0,35
0,3
0,25
0,2
0,5
1
1,5
2
Volume of NaOH( ml)
Fig (3) : Effect of the volume of 1M NaOH on the intensity of color produced for
the reaction (Ranitidine-HCl 10 μg /ml , 1.0 ml of 0.01 M
KMnO4)
545
2,5
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
0.38
Absorbance
0.36
0.34
0.32
0.3
0
10
20
30
40
50
60
Time , minutes
Fig (4) : Effect of time on the oxidation of R-HCl by 0.01M KMnO4
2.5
Absorbance
2
1.5
1
(B)
0.5
(A)
0
200
300
400
500
600
700
Wave length (nm)
Fig (5) : A-absorption spectrum of Ranitidine-HCl before oxidation
B- absorption spectrum of Ranitidine-HCl after oxidation.
Absorbance
1.3
1.1
y = 0.0461 x + 0.7324
R2 = 0.9981
0.9
0.7
0.5
0
2
4
6
μg/ ml Ranitidine- HCl
Fig (6) : Calibration graph for the determenation of
Ranitidine- HCl by the spectrophotometric method
546
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National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
600
(mv)
CL- Intensity (mv)
500
400
300
200
100
0
2
8
4
6
-4
Concentration of Luminol × 10 M
10
12
Fig (7)Effect of concentration of Luminol on the CL- intensity.
600
CL- Intensity (mv)
500
400
300
200
100
0
1
0.5
1.5
Concentration of H2O2 ×10-2M
Fig (8) Effect of concentration of H2O2 on the CL- intens.
547
2
National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
‫المجلد الرابع‬-2006-‫المجلة القطرية للكيمياء‬
600
CL- Intensity
(mv)
550
500
450
400
350
300
250
200
150
100
2.5
5.0
7.5
10.0
Concentration Of H2SO4×10-3M
Fig (9) Effect of Concentration of H2SO4 on the CL-Intensity .
CL- Intensity
(mv)
600
500
400
300
200
100
0
0.2
1
0.6
0.8
0.
+2
4 of Cobalt Co μg /ml
Concentration
1.2
1
Figure (10) Effect of Cobalt concentration on the CL-intensity
CL intensity
(mV)
50
40
Y = 7.7714 X + 0.1333
r =0.9996
30
20
10
0
6
4
2
Conc. Of Ranitidine –HCl µg/ml
Fig(11)calibration graph of Ranitidine –HCl by using FIA-CL method
HCl
548
μg /ml
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National Journal of Chemistry, 2006, Volume 24 ,534-550 ‫والعشرون‬
12. Barnett , N.W.; Hindson , B.J.;
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Martindale, the extra pharmacopoeia
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23. Novakovic , J. J. of chromatography
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