|Year : 2012 | Volume
| Issue : 4 | Page : 237-240
A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations
Shipra Singh, Amrita Mishra, Anurag Verma, Ashoke K Ghosh, Arun K Mishra
Department of Pharmaceutical Chemistry, Central Facility of Instrumentation, College of Pharmacy, IFTM Lodipur-Rajput, Moradabad, India
|Date of Web Publication||14-Dec-2012|
Arun K Mishra
Central Facility of Instrumentation, College of Pharmacy, IFTM, Lodipur-Rajpur, Moradabad
| Abstract|| |
The present study was undertaken to develop a validated, rapid, simple, and low-cost ultraviolet (UV) spectrophotometric method for estimating Etoricoxib (ETX) in pharmaceutical formulations. The analysis was performed on λ max 233 nm using 0.1 M HCl as blank/diluent. The proposed method was validated on International Conference on Harmonization (ICH) guidelines including parameters as linearity, accuracy, precision, reproducibility, and specificity. The proposed method was also used to access the content of the ETX in two commercial brands of Indian market. Beer's law was obeyed in concentration range of 0.1-0.5 μg/ml, and the regression equation was Y = 0.418x + 0.018. The mean accuracy values for 0.1 μg/ml and 0.2 μg/ml concentration of ETX were found to be 99.76 ± 0.52% and 99.12 ± 0.84, respectively, and relative standard deviation (RSD) of interday and intraday was less than 2%. The developed method was suitable and specific to the analysis of ETX even in the presence of common excipients. The method was applied on two different marketed brands and ETX contents were 98.5 ± 0.56 and 99.33 ± 0.44, respectively, of labeled claim. The proposed method was validated as per ICH guidelines and statistically good results were obtained. This method can be employed for routine analysis of ETX in bulk and commercial formulations.
Keywords: Etoricoxib, quality control, UV spectrometry, validation
|How to cite this article:|
Singh S, Mishra A, Verma A, Ghosh AK, Mishra AK. A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations. J Adv Pharm Technol Res 2012;3:237-40
|How to cite this URL:|
Singh S, Mishra A, Verma A, Ghosh AK, Mishra AK. A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations. J Adv Pharm Technol Res [serial online] 2012 [cited 2015 Jan 29];3:237-40. Available from: http://www.japtr.org/text.asp?2012/3/4/237/104715
| Introduction|| |
Chemically Etoricoxib (ETX) is 5-chloro-3-(4-methanesulfonylphenyl)-2-(6-methylpyridin-3-yl) pyridine [Figure 1].  It is a selective COX-2 inhibitor, which belongs to a family of pain killers called non-steroidal anti-inflammatory drugs (NSAIDs). It is mainly used to treat patients suffering from joint pain and swelling caused by osteoarthritis, rheumatoid arthritis, ankylosing spondylitis, and gout. It is also used to reduce swelling and joint stiffness. 
Analysis is an essential step of formulation development, and it must include a simple, reliable, and cost-effective method. Keeping in view this objective, the present work was undertaken to develop and validate simple UV spectrophotometric method for estimation of ETX in dosage formulations.
Earlier methods including high performance liquid chromatography (HPLC), , high performance thin layer chromatography (HPTLC), , liquid chromatography-mass spectrometry (LC-MS),  capillary zone electrophoresis,  and ultra performance liquid chromatography (UPLC)  for quantification of ETX in pharmaceutical dosage forms are reported. These reported methods involve a tedious sample preparation process, costly equipments, as well as time-consuming steps. The long run time of these processes limits their applicability for large number of samples.
Upon literature survey and as per our present knowledge, there is no simple and reliable method for estimation of ETX from pharmaceutical dosage forms as well as in bulk formulation. In this study, a simple UV spectrophotometric method was developed and validated as per International Conference on Harmonization (ICH) guidelines.  This method involves simple instrument and cost-effective solvents, and consumes less time. The reproducibility of the proposed method was high, which accounts this method novel and reliable. The method was also used in the determination of the content of ETX in two marketed ETX products in India.
| Materials and Methods|| |
Instruments and Materials
Schimazdu 1800 double beam UV/Vis spectrophotometer, digital balance (Citizen Co. Mumbai, India), and micropipette (The Modern scientific industries, Meerut, India) were used in this study. ETX was obtained as a gift sample from the Torrent Research Centre, Hyderabad, India. The other chemicals and reagents used were of analytical grade.
Standard Stock Solution
Standard drug solution of ETX was prepared by dissolving 10 mg of ETX in 5 ml 0.1 N HCl in a 10-ml volumetric flask, shaken well, and finally the volume was adjusted to get a solution of concentration of 1 mg/ml. This 1 mg/ml solution was used as a stock solution.
Five milliliters of 1 mg/ml aliquot solution was further diluted up to 50 ml by 0.1 N HCl in a 100-ml volumetric flask and the final volume was adjusted up to 100 ml. This was scanned spectrophotometrically in the wavelength region 190-800 nm to determine the wavelength of maximum (λmax) absorption. The λmax was found to be 233 nm against blank [Figure 2]. From 1 mg/ml stock solution, the serial dilution pattern was followed to obtain aliquots of 0.1-0.5 μg/ml concentration. The calibration curve was plotted between concentration and absorbance. The optical characteristics of different aliquots are presented in [Table 1].
Sample Solution Preparations
The proposed method was applied on two different commercial brands of ETX. Twenty tablets of each brand were weighed and powdered. Ten milligrams of ETX powder equivalents was weighed and transferred in a 10-ml volumetric flask by diluting it with 10 ml 0.1 N HCl. After a continuous shaking for 10 min, the solutions were filtered through Whatman filter paper separately. The filtrate was further suitably diluted in order to get 0.2 μg/ml concentration. Against a blank solution, the absorbance was measured at 233 nm wavelength. Finally, employing the calibration curve and linear equation, the concentration was calculated. Determination of accuracy was done by % addition method and is presented in [Table 2]. Amount of drug estimated through this method is presented in [Table 2].
|Table 2: Determination of accuracy (by percentage recovery method) and precision|
Click here to view
| Results and Discussion|| |
The linearity of the drug was obtained for 0.1-0.5 μg/ml concentration range of ETX. The calibration curve was obtained by plotting absorbance versus concentration and linear regression analysis was performed to get linear equation. The linear equation found was y = 0.418x + 0.018 and r 2 was 0.997. The calibration curve was found to be linear in stated concentration.
Accuracy of the method was estimated by standard addition recovery method. In this, known amount of standard ETX was added to pre-analyzed sample.  This was done for 0.1 μg/ml, 0.2 μg/ml, and performed in triplicate. The accuracy values for 0.1 μg/ml and 0.2 μg/ml concentration of ETX were found to be 99.76 ± 0.52 and 99.12 ± 0.84%, respectively [Table 2].
The precision of the assay was determined by repeatability (intraday) and intermediate precision (interday) and reported as % relative standard deviation (RSD).  For this, 0.1 μg/ml and 0.2 μg/ml concentration solution was measured three times in day and the same was measured in the next 3 days. The %RSD was calculated [Table 2].
Robustness of the method was determined by carrying out the analysis under different temperature conditions, i.e. at room temperature and at 18°C.  The respective absorbance of 0.3 μg/ml was noted and the result was indicated as %RSD [Table 3].
The ruggedness of the method was determined by carrying out the analysis by different analysts and the respective absorbance of 0.3 μg/ml was noted. The result was indicated as %RSD [Table 4].
Limit of Detection and Limit of Quantification
The limit of detection (LOD) and limit of quantification (LOQ) for ETX were determined by using standard deviation of response and slope.  The LOD and LOQ values are presented in [Table 5].
The stability of ETX in 0.1 N HCl solution was studied by the developed method. Sample solutions (0.3 μg/ml) were prepared in triplicate and heated to maintain 50°C and 60°C for 60 min.  The absorbance data of these samples reveled information about the stability of ETX [Table 6].
Determination of Active Ingredients in Different Brands of Tablets
The proposed and validated method was applied to estimate the amount of active ingredient, ETX, in two different brands of tablets using 20 tablets in each batch. Results of quantitative analysis are presented in [Table 7]. The findings of analysis suggest that both the marketed formulations fulfilled the % amount requirement (98-102%) with respect to labeled claim.
| Conclusion|| |
The developed method was found to be simple, rapid, cost-effective, and reproducible, with high accuracy and precision value. The parameters were validated as per ICH guidelines. The satisfactory findings of the work suggest that the method may be applied for quantitative estimation of ETX from bulk and pharmaceutical dosage formulations. This method may also be used in routine quality-control aspects.
| Acknowledgment|| |
Authors would like thanks to Prof. R.M.Dubey (Honourable Vice-Chancellor of IFTM University) for his kind support.
| References|| |
|1.||Muralidhar S, Rao GD, Murthy MK, Kumar KK, Teja KK. Enhancement of dissolution rate of Etoricoxib through solid dispersion technique. J Appl Pharm Sci 2011;05:129-32. |
|2.||Moraes BM, Amaral BC, Morimoto MS, Vieira LG, Perazzo FF, Carvalho JC. Anti-inflammatory and analgesic actions of etoricoxib (an NSAID) combined with misoprostol. Inflammopharmacology 2007;15:175-8. |
|3.||Patel HM, Suhagia BN, Shah SA, Rathod IS. Determination of etoricoxib in pharmaceutical formulations by HPLC method. Indian J Pharm Sci 2007;69:703-5. |
|4.||Thimmaraju MK, Rao V, Hemanth K, Siddartha P. RP HPLC method for the determination of Etoricoxib in bulk and pharmaceutical formulations. Der Pharmacia Lettre 2011;3:224-31 |
|5.||Rajmane VS, Gandhi SV, Patil UP, Sengar MR. High-performance thin-layer chromatographic determination of Etoricoxib and Thiocolchicoside in combined tablet dosage form. J AOAC Int 2010;93:783-6. |
|6.||Baheti KG, Shaikh S, Shah N, Dehghan MH. Validated simultaneous estimation of Paracetamol and Etoricoxib in bulk and tablet by HPTLC method. Inter J Res Pharma Biomed Sci 2011;2:672-75. |
|7.||Brum L Jr, Fronza M, Ceni DC, Barth T, Dalmora SL. Validation of liquid chromatography and liquid chromatography/tandem mass spectrometry methods for the determination of Etoricoxib in pharmaceutical formulations. J AOAC Int 2006;89:1268-75. |
|8.||Dalmora SL, Sangoi Mda S, da Silva LM, Macedo RO, Barth T. Validation of a capillary zone electrophoresis method for the comparative determination of Etoricoxib in pharmaceutical formulations. J Sep Sci 2008;31:169-76. |
|9.||Vora DN, Kadav AA. Separation of etoricoxib and its degradation products in drug substance using UPLC TM. Eurasian J Ana Chem 2007;2:182-9. |
|10.||ICH. Q2A validation of analytical procedure-Guidelines, Methodology International Conference on Harmonization.Steering Committee, Geneva: 1994. |
|11.||Acharjya SK, Mallick P, Panda P, Kumar KR, Annapurna MM. Spectrophotometric methods for the determination of Letrozole in bulk and pharmaceutical dosage forms. J Adv Pharm Technol Res 2010;1:348-53. |
|12.||Arora G, Malik K, Singh I, Arora S, Rana V. Formulation and evaluation of controlled release matrix mucoadhesive tablets of domperidone using Salvia plebeian gum. J Adv Pharm Technol Res 2011;2:163-9. |
|13.||International Conference on Harmonization, Draft Guideline on Validation Procedure, Definition and Terminology. Federal Register. 1995;60:11260-2. |
|14.||Shah GR, Ghosh C, Thaker BT. Determination of pregabalin in human plasma by electrospray ionisation tandem mass spectroscopy. J Adv Pharm Technol Res 2010;1:354-7. |
|15.||Argekar AP, Sawant JG. Determination of Cisapride in pharmaceutical dosage forms by reversed phase liquid chromatography. J Pharm Biomed Anal 1999;21:221-6. |
|16.||Mishra AK, Kumar A, Mishra A. Development and validation of UV spectrophotometric method for estimation of diphenhydramine hydrochloride in soft gelatin capsule. Intern J Pharm Res 2010;1:22-6. |
[Figure 1], [Figure 2]
[Table 1], [Table 2], [Table 3], [Table 4], [Table 5], [Table 6], [Table 7]