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Diclofenac Spectrofotometric - Grupa 21
Diclofenac Spectrofotometric - Grupa 21
105-108, 1995
Copyright ~3 1994 Elsevier Science Ltd
Pergamon 0039-9140(94)00224-X Printed in Great Britain. All rights reserved
0039-9140/95 $9.50 + 0.00
SPECTROPHOTOMETRIC DETERMINATION OF
DICLOFENAC SODIUM WITH METHYLENE BLUE
Summary--A sensitive spectrophotometric method was established for the determination of Diclofenac
sodium (DS) with Methylene Blue (MB) as analytical reagent. It was found that DS reacts with an excess
of MB in the pH range 9.2-9.4, to form a chloroform-extractable blue ion-association complex. Good
agreement with Beer's law was found in the range of DS concentrations of 0.8~.4/ag/ml with a detection
limit of 0.37 pg/ml. The method was applied for the determination of DS in various tableted forms with
a good precision.
Procedure
EXPERIMENTAL
Aliquots of DS solution were transferred into
Apparatus
a series of 125 ml separating funnels; then 5 ml
A Beckman DU-65 single beam spectropho- of MB solution and 1 ml of buffer (pH 9.4) was
tometer with 10 m m glass cells was used for the added. The total volume of the aqueous phase
absorbance measurements. The p H measure- was adjusted to 10 ml with water. Chloroform
ments were made with a Corning Model 12 (10 ml) was added and the contents shook for
exactly 5 min, the separated chloroform layer
*Author to whom the correspondence should be addressed. was collected in a 25 ml volumetric flask. A new
105
106 J. C. BOTELLO and G. Pi~REZ-CABALLERO
<•CHzCOONa
to 50 ml with deionized water and treated as
described above for the standard drug solution.
NH C l ~
0.9
A
B zq
S 0.6
O
R e i
B i i
A
N
C e" I
E 0.3 II
..... o°,"
° ° . . ° - °
0.0 I I
400 500 600 700
WAVELENGTH(nm)
Fig. 2. The absorption spectra of the blank reagent (---), and DS-MB ( ) complex formed in the
aqueous 0.05M NH+/NH3 buffer containing 5 x 10-4M MB and extracted with chloroform.
Determination of Diclofenac sodium with Methylene Blue 107
0.7
A
B
$ 0.6
O
R
B
A
N
C 0.5
E
I I I I I
8.0 9.0 10.0 11.0 12.0
pH
Fig. 3. Variation in absorbance of the DS-MB complex, fonned in aqueous 0.05M NH+/NH3 buffer
containing 5 x 10-4M MB at different pH values (aborbances were obtained at 2653nm)"
The extent of the extraction of the ion-associ- produced a constant absorbance. An ionic
ated complex was found to be affected by the strength of 0.025M was produced by the buffer.
MB concentration. To establish the optimum
MB concentration the solution absorbances Linearity
were plotted as a function of MB concentration
(Fig. 4). The absorbance of the system increased A calibration curve was obtained under opti-
in the range of 1-3.5 x 10-4M MB and the m u m conditions (pH 9.4; 5 x 10-4M MB; ionic
absorbance was practically constant in a range strength 0.025M), absorbance responses were
of 4-6 x 10-4M MB, hence a concentration of linear in relation to the calculated concentration
5.0 x 10-4M MB was used as the optimum of DS over the range 0.8-6.4 mcg/mi
concentration. The excess of MB in this system (2.5 x 10-6-2.5 x 10-SM). The equation for
was 25-200 times the concentration of DS. one representative calibration curve is:
Two extractions were necessary to achieve a A = ( - 0 . 0 1 9 1 + 0.0423) + (0.1789 + 0.0105)C,
quantitative recovery of the complex. Ab-
sorbances of the separated extracts were stable where A and C correspond to absorbance
for at least 1 hr. A shaking time of 5 min and DS calculated concentration (pg/mi),
1.3.
X I .-.'4
1.2'
A
B
S
1.1'
o
R
B
1.0,
A
N
C
E 0.9
0.8 ¸
0.7 I ! I I I i
0 1.0 2.0 3.0 4.0 S.0 6.0
[MB| (M X 10 -4)
Fig. 4. Variation in absorbance of the DS-MB complex, formed in aqueous 0.05M NH~/NH~ buffer
containing different concentrations of MB (absorbances were obtained at 2653,m).
108 J.C. BOTELLOand G. I~REZ-CABALLERO
Table 1. Comparison of sensitivity parameters of the differ- o f the m a t r i x effect over the absorbances
ent spectrophotometric methods for the determination of measurements.
Diclofenac sodium
Sandell Detection CONCLUSIONS
Analytical sensitivity limit
reagent (rag/cm 2) (mcg /ml) T h e p r o p o s e d m e t h o d is economical, simple,
Copper acetate 0.01026 1.00 rapid, precise a n d sensitive. The use o f M B as
Methylene Violet -- 72.00 a n a l y t i c a l reagent p r o v i d e s a fairly higher sensi-
Methylene Blue 0.006 0.37
tivity c o m p a r e d with o t h e r similar reagents such
as M e t h y l e n e Violet.
Table 2. Determination of Diclofenac sodium in different
tableted dosage Acknowledgements--We thank Dr Ignacio Gonzfilez for his
collaboration in this project. J. C. Botello acknowledges the
Labeled amount Amount found scholarship from CONACYT.
Drug (mg ) (rag)
Flenaken 100.00 101.45 + 0.42
Voltaren Retard 100.00 101.35 _+0.13 REFERENCES
Voltaren 50.00 49.97 _+0.15
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