Estimation of Paracetamol and Aceclofenac in Tablet Formulation by Ratio Spectra Derivative Spectroscopy

Indian Journal of Pharmaceutical Sciences 635 September October 2008 EL, Gilman AG, editors. Goodman and Gilman’s the Pharmacological Basis of Therapeutics. 10th ed. New York: McGraw-Hill; 2001. p. 843-70. 7. British Pharmacopoeial Commission. British Pharmacopoeia. London: Stationery Offi ce Books; 2004. p. 1457. 8. Khanna R, Agarwal SP, Ahuja A. Preparation and evaluation of mucoadhesive buccal fi lms of clotrimazole for oral Candida infections. Indian J Pharm Sci 1997;59:299-305. 9. Patil JS, Rao KP. Design and evaluation of mucoadhesive buccal patches of diclofenac sodium. Indian J Pharm Sci 2003;65:420-3 10. Khurana R, Ahuja A, Khar AK. Development and evaluation of mucoadhesive films of miconazole nitrate. Indian J Pharm Sci 2002;62:447-53. 11. Nafee NA, Ismail FA. Design and characterization of mucoadhesive buccal patches containing cetyl pyridinium chloride. Acta Pharm 2003;53:199-212. 12. Panigrahi L, Pattinaik S, Ghosal SK. Design and characterization of mucoadhesive buccal patches of diclofenac sodium. Indian J Pharm Sci 2005;67:319-25. 13. Shaila L, Pandey S, Udupa N. Design and evaluation of matrix type and membrane controlled transdermal delivery systems of nicotine suitable for use in smoking cessation. Indian J Pharm Sci 2006;68:17984. 14. Chowdary KP, Girish KK, Rao DG. Spectrophotometric determination of nitrendipine in pharmaceutical dosage forms. Indian Drugs 1998;35:645-7.

Aceclofenac (AFC) is {o-(2,6-dichloroanilino)phenyl} acetate glycolic acid ester with antiinfl ammatory and analgesic properties 1 .Paracetamol (PAR) chemically is 4-hydroxy acetanilide 2 .Several analytical methods are reported for determination of AFC and PAR in bulk and pharmaceutical dosage formulations as a single component as well as in combination with other drugs.Recently UV spectrophotometric method for simultaneous estimation of aceclofenac and paracetamol in a combined tablet dosage form has been reported 3 .Extensive literature survey revealed that no method is available for simultaneous estimation of AFC and PAR in combined dosage form by ratio spectra derivative spectroscopy [4][5][6] .Aim of present work was to develop simple, economical, reproducible and rapid method for simultaneous estimation of binary drug formulation.
The instrument used in the present study was JASCO double beam UV/Vis spectrophotometer (Model UV-530) with fixed slit width 2 nm connected to a computer with spectra manager software.All weighing were done on electronic balance (Shimadzu AY 120).AFC and PAR were obtained from Concept Pharmaceuticals Pvt. Ltd. and Cipla Ltd., respectively, which were used as such without further purifi cation.All chemicals used in spectrophotometric analysis were of analytical grade.Tablets of Aceroc-P (Wockhardt Ltd.) labeled to contain AFC 100 mg and PAR 500 mg were procured from the local market.
Standard stock solution was prepared by dissolving 50 mg of PAR and AFC separately in 50 ml of methanol to get concentration of 1 mg/ml.Ten ml of stock solutions were further diluted to 100 ml with phosphate buffer (pH-7, prepared as per IP) to get a working standard solution of concentration 100 μg/ml of each drug.For commercial formulation analysis twenty tablets were weighed accurately and powdered.Powder equivalent to 50 mg of PAR was weighed and transferred to 50 ml volumetric fl ask; in the same fl ask 40 mg of pure AFC drug was added and dissolved in methanol by shaking the flask for 10 min.The solution was fi ltered through Whatman fi lter paper No. 41 and fi rst few ml were rejected.10 ml of this fi ltrate was further diluted to 100 ml with phosphate buffer pH-7.Two millilitres of this solution was further diluted to 10 ml to get fi nal concentration of 20 μg/ml of each drug.Spectra was recorded and processed separately to determine concentration of each drug.
Salinas et al 7 developed a ratio spectra derivative spectroscopic method based on dividing the spectrum for a mixture into the standard spectra for each of the analyses and driving the quotient to obtain a spectrum that is independent of the analyte concentration used as a divisor.The use of standardized spectra as divisors minimizes experimental errors and background noise.Easy measurements on separate peaks, higher values of the analytical signals and no need to work only at zero-crossing points (sometimes coexisting compounds have no maximum or minimum at these wavelengths) are advantages for ratio spectra derivative spectrophotometry in comparison with the zero-crossing derivative spectrophotometry.Also, the presence of a lot of maxima and minima in ratio spectra derivative data was another advantage, since these wavelengths give an opportunity for the determination of these compounds in the presence of other active compounds and excipients that possibly interfered with the assay.Using appropriate dilutions of standard stock solution the two solutions were scanned separately.The ratio spectra of different AFC standards at increasing concentrations was obtained by dividing each with the stored spectrum of the standard solution of PAR (30 μg/ml) by computer aid are shown in fig. 1 (a) and the first derivative of these spectra traced with the interval of = 13 nm (the influence of Δλ for the first derivative of the ratio spectra was tested to obtain the optimum wavelength interval, Δλ= 13 nm was considered to be suitable) are illustrated in fi g. 1 (b).Wavelength 268 nm (minima) was selected for the quantifi cation of AFC in AFC+PAR mixture.The ratio and ratio derivative spectra of the solutions of PAR at different concentrations traced with the interval of = 13 nm by using the standard spectrum of AFC (10 μg/ ml) as divisor by computer aid are demonstrated in fig. 2 (a) and (b), respectively.Wavelength 256 nm (maxima) was selected for the quantification of PAR in AFC+PAR mixture.Measured analytical signals at these wavelengths were proportional to the concentrations of these drugs.found in the range 10-50 μg/ml with high correlation coeffi cients for both the drugs.Six replicate readings of drug solution were taken to study the precision of method.%RSD was found to be less than 1.5, indicating reproducibility.For recovery study different volumes of standard solution was added to the fi xed volume of sample solution.The total amount of drug added was determined by proposed method.Results of recovery studies are shown in Table 1.

Vengurlekar, et al.: Prescribing pattern of antidiabetic drugs
Diabetes mellitus is a metabolic disorder characterized by hyperglycemia, glycosuria, and sometimes ketonemia.The present study was carried out to assess prescribing practice and general trend of diabetes among patients at the Bombay Hospital, Indore.Prescriptions and complete records of diabetic patients were monitored and data was fi led as per WHO prescription proforma.The study revealed that prescription of metformin (27%) and glimepiride (22.60%) were found to be maximum among various available antidiabetic drugs.Category wise the maximum prescribed drugs are glimepride (22.60%, sulfonylurea category), metformin (27%, biguanide category) and pioglitazones (13.90%, glitazone category).Insulin prescription was found to be very less (4.5%).Combination of metformin and glimepiride (20.86%) was prescribed most commonly.Most common disease associated with

Fig. 1 :Fig. 2 :
Fig. 1: Ratio and fi rst derivative of the ratio spectra AFC and PAR Ratio spectra (a) and fi rst derivative of the ratio spectra (b) of 10-50 μg/ml solution of AFC when 30 μg/ml solution of PAR is used as divisor (=13 nm).