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

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EL, Gilman AG, editors. Goodman and Gilman’s the Pharmacological mucoadhesive buccal patches of diclofenac sodium. Indian J Pharm Basis of Therapeutics. 10th ed. New York: McGraw-Hill; 2001. p. Sci 2005;67:319-25. 843-70. 13. Shaila L, Pandey S, Udupa N. Design and evaluation of matrix type 7. British Pharmacopoeial Commission. British Pharmacopoeia. London: and membrane controlled transdermal delivery systems of nicotine Stationery Ofﬁ ce Books; 2004. p. 1457. suitable for use in smoking cessation. Indian J Pharm Sci 2006;68:179- 8. Khanna R, Agarwal SP, Ahuja A. Preparation and evaluation of 84. mucoadhesive buccal ﬁ lms of clotrimazole for oral Candida infections. 14. Chowdary KP, Girish KK, Rao DG. Spectrophotometric determination Indian J Pharm Sci 1997;59:299-305. of nitrendipine in pharmaceutical dosage forms. Indian Drugs 9. Patil JS, Rao KP. Design and evaluation of mucoadhesive buccal 1998;35:645-7. 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. Accepted 1 October 2008 11. Nafee NA, Ismail FA. Design and characterization of mucoadhesive Revised 4 February 2008 buccal patches containing cetyl pyridinium chloride. Acta Pharm Received 10 April 2007 2003;53:199-212. 12. Panigrahi L, Pattinaik S, Ghosal SK. Design and characterization of Indian J. Pharm. Sci., 2008, 70 (5): 631-635

A. D. NIKAM, SAMPADA S. PAWAR AND S. V. GANDHI* A. I. S. S. M. S. College of Pharmacy, Kennedy Road, Near R. T. O., Pune-411 001, India

Gandhi, et al.: Spectroscopic estimation of Paracetamol and Aceclofenac

A new sensitive, simple, rapid and precise method for simultaneous estimation of paracetamol and aceclofenac in combined tablet dosage form has been developed. The method is based on ratio derivative spectrophotometry. The amplitude in ﬁ rst derivative of the ratio spectra at 256 nm and 268 nm (minima) were selected to determine paracetamol and aceclofenac in combined formulation. The method showed good linearity, accuracy and reproducibility. Results of analysis were validated statistically and by recovery studies.

Key words: Aceclofenac, paracetamol, ratio spectra derivative spectroscopy

Aceclofenac (AFC) is {o-(2,6-dichloroanilino)phenyl} of present work was to develop simple, economical, acetate glycolic acid ester with antiinﬂ ammatory and reproducible and rapid method for simultaneous analgesic properties1. Paracetamol (PAR) chemically estimation of binary drug formulation. is 4-hydroxy acetanilide2. Several analytical methods are reported for determination of AFC and PAR The instrument used in the present study was JASCO in bulk and pharmaceutical dosage formulations double beam UV/Vis spectrophotometer (Model as a single component as well as in combination UV-530) with fixed slit width 2 nm connected to with other drugs. Recently UV spectrophotometric a computer with spectra manager software. All method for simultaneous estimation of aceclofenac weighing were done on electronic balance (Shimadzu and paracetamol in a combined tablet dosage AY 120). AFC and PAR were obtained from Concept form has been reported3. Extensive literature survey revealed that no method is available for simultaneous Pharmaceuticals Pvt. Ltd. and Cipla Ltd., respectively, estimation of AFC and PAR in combined dosage which were used as such without further puriﬁ cation. form by ratio spectra derivative spectroscopy4-6. Aim All chemicals used in spectrophotometric analysis were of analytical grade. Tablets of Aceroc-P *For correspondence (Wockhardt Ltd.) labeled to contain AFC 100 mg and E-mail: [email protected] PAR 500 mg were procured from the local market.

September - October 2008 Indian Journal of Pharmaceutical Sciences 635 www.ijpsonline.com Standard stock solution was prepared by dissolving be suitable) are illustrated in fi g. 1 (b). Wavelength 50 mg of PAR and AFC separately in 50 ml of 268 nm (minima) was selected for the quantifi cation methanol to get concentration of 1 mg/ml. Ten ml of AFC in AFC+PAR mixture. The ratio and ratio of stock solutions were further diluted to 100 ml derivative spectra of the solutions of PAR at different with phosphate buffer (pH-7, prepared as per IP) concentrations traced with the interval of = 13 to get a working standard solution of concentration nm by using the standard spectrum of AFC (10 μg/ 100 μg/ml of each drug. For commercial formulation ml) as divisor by computer aid are demonstrated analysis twenty tablets were weighed accurately and in fig. 2 (a) and (b), respectively. Wavelength 256 powdered. Powder equivalent to 50 mg of PAR was nm (maxima) was selected for the quantification weighed and transferred to 50 ml volumetric fl ask; in of PAR in AFC+PAR mixture. Measured analytical the same fl ask 40 mg of pure AFC drug was added signals at these wavelengths were proportional to the and dissolved in methanol by shaking the flask for concentrations of these drugs. 10 min. The solution was fi ltered through Whatman fi lter paper No. 41 and fi rst few ml were rejected. 10 Under experimental conditions described linearity was ml of this fi ltrate was further diluted to 100 ml with 15 phosphate buffer pH-7. Two millilitres of this solution ] was further diluted to 10 ml to get fi nal concentration 10 para of 20 μg/ml of each drug. Spectra was recorded and /A processed separately to determine concentration of Aceclo 5 [A each drug. 0 250 260 280 300 320 340 350 Salinas et al7 developed a ratio spectra derivative (a) Wavelength [nm] spectroscopic method based on dividing the spectrum 0.5

for a mixture into the standard spectra for each of the ] 0 para

analyses and driving the quotient to obtain a spectrum /A -0.5

that is independent of the analyte concentration used Aceclo [A as a divisor. The use of standardized spectra as λ -1 divisors minimizes experimental errors and background d/dλ -1.2 250260 280 300 310 noise. Easy measurements on separate peaks, higher (b) Wavelength [nm] values of the analytical signals and no need to Fig. 1: Ratio and ﬁ rst derivative of the ratio spectra AFC and PAR work only at zero-crossing points (sometimes co- Ratio spectra (a) and ﬁ rst derivative of the ratio spectra (b) of 10-50 existing compounds have no maximum or minimum μg/ml solution of AFC when 30 μg/ml solution of PAR is used as divisor (=13 nm). at these wavelengths) are advantages for ratio spectra derivative spectrophotometry in comparison with the 15 zero-crossing derivative spectrophotometry. Also, 10 the presence of a lot of maxima and minima in ]

ratio spectra derivative data was another advantage, Aceclo since these wavelengths give an opportunity for the / A 5 para determination of these compounds in the presence of [ A 0 210250 300 350 other active compounds and excipients that possibly (a) Wavelength [nm] interfered with the assay. Using appropriate dilutions 1 of standard stock solution the two solutions were ] 0.5 scanned separately. The ratio spectra of different AFC Aceclo / A standards at increasing concentrations was obtained 0 para

by dividing each with the stored spectrum of the [ A λ -0.5

standard solution of PAR (30 μg/ml) by computer d/dλ -1 aid are shown in fig. 1 (a) and the first derivative 210 250 300 350 (b) of these spectra traced with the interval of = 13 Wavelength [nm] nm (the influence of Δλ for the first derivative of Fig. 2: Ratio and ﬁ rst derivative of the ratio spectra PAR and AFC Ratio spectra (a) and ﬁ rst derivative of the ratio spectra (b) of 10 -50 the ratio spectra was tested to obtain the optimum μg/ml solution of PAR when 10 μg/ml solution AFC of is used as wavelength interval, Δλ= 13 nm was considered to divisor (= 13 nm).

636 Indian Journal of Pharmaceutical Sciences September - October 2008 www.ijpsonline.com

TABLE 1: RECOVERY STUDIES OF AFC AND PAR Level of % Mean Standard % RSD Standard % Recovery Recovery* Deviation Error AFC PAR AFC PAR AFC PAR AFC PAR 50 100.1 100.06 0.0866 0.07637 0.0865 0.0763 0.0499 0.044 100 100.05 99.97 0.0854 0.08326 0.0853 0.0832 0.0493 0.048 150 99.756 99.986 0.4045 0.12055 0.4054 0.1205 0.2335 0.0395 *Average of three determinations, RSD is relative standard deviation found in the range 10-50 μg/ml with high correlation ed. London: The Pharmaceutical Press; 1993. p. 2. coefﬁ cients for both the drugs. Six replicate readings 2. British Pharmacopoeial Commission. British Pharmacopoeia. Vol. I. International ed. London: HMSO Publication; 1993. p. 483. of drug solution were taken to study the precision 3. Nikam AD, Pawar SS, Gandhi SV. Simultaneous spectrophotometric of method.% RSD was found to be less than 1.5, estimation of aceclofenac and Paracetamol. Asian J Chem 2007;19:5075- indicating reproducibility. For recovery study different 80. 4. Dinc E. The spectrophotometric multicomponent analysis of ternary volumes of standard solution was added to the ﬁ xed mixture of ascorbic acid, acetyl salicylic acid and paracetamol by volume of sample solution. The total amount of drug double divisor ratio spectra derivative and ratio spectra zero crossing added was determined by proposed method. Results method. Talanta 1999;48:1945-57. 5. Erk N. Comparison of spectrophotometric and an LC method for of recovery studies are shown in Table 1. the determination perindropil and indapamide in pharmaceutical formulations. J Pharm Biomed Anal 2001;26:43-52. 6. Abdel AY, Sayed El, Najeb A, Salem El. Recent development of ACKNOWLEDGMENTS derivative spectrophotometry and their analytical applications. Anal Sci 2005;21:595-600. The authors thank the Concept Pharmaceutical Pvt. Ltd., 7. Salinas F, Berzas-Nevado JJ, Espinosa MA. A new spectrophotometric Aurangabad and Cipla Ltd., Mumbai for providing gift method for quantitative multicomponent analysis resolution of mixtures sample of ACF and PAR respectively. Thanks are also of salicylic and salicyluric acids. Talanta 1990;37:347-51. due to the principal, Dr. K. G. Bothara, for providing infrastructure facilities. Accepted 1 October 2008 REFERENCES Revised 12 February 2008 Received 30 January 2007 1. Reynolds JE, Prasad BA. Martindale – The Extra Pharmacopoeia. 30th Indian J. Pharm. Sci., 2008, 70 (5): 635-637

Prescribing Pattern of Antidiabetic Drugs in Indore City Hospital

SUDHA VENGURLEKAR*, PRERNA SHUKLA, P. PATIDAR, R. BAFNA AND S. JAIN Smriti College of Pharmaceutical Education, 4/1, Piplia Kumar Kakad Mayakhedi Road, Indore-452 001, India

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

*For correspondence E-mail: [email protected]

September - October 2008 Indian Journal of Pharmaceutical Sciences 637