Spectrophotometric determination of diclofenac in pharmaceutical preparations assisted by microwave oven
Main Article Content
Abstract
In this work, an effective and low-cost method for the determination of sodium or potassium
diclofenac is proposed in its pure form and in their pharmaceutical preparations. The method is based on the
reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium. This reaction
was accelerated by irradiating of reactional mixture with microwave energy (1100 W) during 27 seconds,
producing a charge transfer complex with a maximum absorption at 535 nm. The optimal reaction conditions
values such as reagent concentration, heating time and stability of the reaction product were determined.
Beer’s law is obeyed in a concentration range from of 1.25x10 -4 to 2.00x10 -3 mol l -1 with a correlation
coefficient of 0.9993 and molar absorptivity of 0.49 x10 3 l mol -1 cm -1 . The limit of detection (LOD) was
1.35x10 -5 mol l -1 and the limit of quantification (LOQ) was 4.49x10 -5 mol l -1 . In the presence of the common
excipients, such as glucose, lactose, talc, starch, magnesium stearate, sodium sulphite, titanium dioxide,
polyethyleneglycol, polyvinylpirrolidone, mannitol and benzilic alcohol no interferences were observed.
The analytical results obtained by applying the proposed method compare very favorably with those given
by the United States Pharmacopeia standard procedure.
Metrics
Article Details
This work is licensed under a Creative Commons Attribution 4.0 International License.
The corresponding author transfers the copyright of the submitted manuscript and all its versions to Eclet. Quim., after having the consent of all authors, which ceases if the manuscript is rejected or withdrawn during the review process.
When a published manuscript in EQJ is also published in other journal, it will be immediately withdrawn from EQ and the authors informed of the Editor decision.
Self-archive to institutional, thematic repositories or personal webpage is permitted just after publication. The articles published by Eclet. Quim. are licensed under the Creative Commons Attribution 4.0 International License.
References
R.T. Sane, R.S. Samant, V.G. Nayak, Drug Dev. Ind.
Pharm. 13 (1987) 1307.
J. Klimes, J. Sochor, P. Dolezal, J. Körner, Int. J. Pharm.
(2001) 153.
N. Beaulieu, E.G. Loveringe, J. Lefrancois, H. Ong, J.
Assoc. Off. Anal. Chem. 73 (1990) 698.
M.S. Aurora-Prado, M. Steppe, M.F.M. Tavares, E.R.M.
Kedor-Hackmann, M.I.R.M. Santoro, J. Assoc. Off. Anal.
Chem. 85 (2002) 333.
W.R. Jin, J. Zhang, , J. Chromatogr. A. 868 (2000) 101.
M.E. Abdel-Hamid, L. Novotony, H. Hamza, J. Pharm.
Biomed. Anal. 24 (2001) 587.
R. Bucci, A.D. Magri, A.L. Magri, J. Therm. Anal. Calorim.
(2000) 369.
S.A. Abdel Fattah, S.Z. El-Khateeb, S.A. Abdel Razeg,
M.S. Tawakkol, Spectrosc. Lett. 21 (1988) 533.
J.C. Botello, G.P. Caballero, Talanta 42 (1995) 105.
M.S. Bhatia, S.R. Dhaneshwar, The Eastern Pharmacist
(1995) 133.
Y.K. Agrawal, K. Shivramchandra, J. Pharm. Biomed.
Anal. 9 (1991) 97.
S. AgatonovicKustrin, L. Zivanovic, D. Radulovic, M.
Vasiljevic, Analyst 116 (1991) 753.
C.S.P. Sastry, A.S.R.P. Tipirneni, M.V. Suryanaryana,
Analyst 114 (1989) 513.
B.V. Kamath, K. Shivram, Anal. Lett. 26 (1993) 903.
S. AgatonovicKustrin, L. Zivanovic, M.Zecevic, D.
Radulovic, J. Pharm. Biomed. Anal. 16 (1997) 146.
R. Bucci, A.D. Magri, A.L. Magri, Fres. J. Anal. Chem.
(1998) 577.
M.L.F. Cordova, P.O. Barrales, A.M. Diaz, Anal. Chim.
Acta 369 (1998) 262.
B.V. Kamath, K. Shivram, G.P. Oza, S. Vangani. Anal.
Lett. 26 (4) (1993) 665.
R.S. Mulliken, J. Am. Chem. Soc. 72 (1950) 600.
R.S. Mulliken, J. Am. Chem. Soc. 74 (1952) 811.
R.S. Mulliken, J. Phys. Chem. 56 (1952) 801.
M.A. Korany, M.A. Wahby, Analyst 104 (1979) 146.
L.I. Bebawy, N. El-Kousy, J.K. Suddik, M. Shokry, J.
Pharm. Biomed. Anal. 21 (1999) 133.
B.V. Kamath, K. Shivram, S. Vangani, Anal. Lett. 25
(1992) 2239.
H.E. Abdellatef, J. Pharm. Biomed. Anal. 17 (1998) 1267.
H. Salem, J. Pharm. Biomed. Anal. 29 (2002) 527.
R.E. Smith, W.R. Davis, Anal. Chem. 56 (1984) 2345.
F. Feigl, V. Gentil, C. Stark-Mayer, Mikrochim. Acta 51
(1957) 341.
F. Feigl, Spot Tests in Organic Analysis, 7th ed., Elsevier,
Amsterdam, 1966, pp. 249 and 407.
E.A. Ibrahim, A.S. Issa, M.A. Abdel-Salam, M.S.
Mahrous, Talanta 30 (1983) 531.
A. Abu-Samra, J.S. Morris, S.R. Koirtyohann, Anal. Chem.47 (1975) 1475.
L.A. Fernando, W.D. Heavner, C.C. Gabrielli, Anal.
Chem. 58 (1986) 511.
L.B. Fischer, Anal. Chem. 58 (1986) 261.
F. Smith, B. Cousins, J. Bozic, W. Flora, Anal. Chim. Acta
(1985) 243.
H.M. Kingston, L.B. Jassie, Anal. Chem. 58 (1986) 2534.
T. Hirose, B.G. Hopek, Z. Wang, R. Yusa, B.W. Baldwin,
Tetrahedron Lett. 44 (2003) 1831.
United States Pharmacopeia National Formulary, USP
, NF 20, Rockville, 2002, p. 554.
H.M. Kingston, P.J. Walter, S. Chalk, E. Lorentzen, D.
Link, in: H.M. Kingston, S.J. Haswell (Eds.), Microwave -
Enhanced Chemistry - Fundamentals, Sample Preparation and
Applications, ACS, Washington, 1997, p. 772.
A. Morales-Rubio, J. Cerezo, A. Salvador, M. De la
Guardia, Microchem. J. 47 (1993) 270.
L. Pezza, H.R. Pezza, C.B. Melios, A. Leandro, A.G.
Tininis, Anal. Lett. 33 (2000) 2901.
G.L Long, J.D.Winefordner, Anal. Chem. 55 (1983) 712A.