Estimation of Piroxicam in Tablet Dosage Form by using UV-Vis. Spectrophotometer
Sunil Singh*, Jay Ram Patel, Sarita Kare
Department of Pharmaceutical Chemistry, Oriental College of Pharmacy, Bhopal, M.P.
*Corresponding Author E-mail: rssunil29@rediffmail.com rssunil29@gmail.com
ABSTRACT:
A simple, accurate, sensitive and precise Ultraviolet spectrophotometric method has been developed for the determination of Piroxicam in tablet dosage form. The solutions of standard and sample were prepared in methanol. In the UV specrophotometric method, the quantitative determination of the drug was carried at 335 nm and the linearity range was found to be 2-12 μg/ml. The calibration graphs constructed at their wavelength of determination were found to be linear for specrophotometric methods. The proposed methods have been extensively validated statistically that included parameters such as linearity, accuracy, precision, LOD, LOQ, recovery and robustness. There was no significant difference between the performance of the proposed method regarding the mean values and standard deviations. The described methods can be readily utilized for analysis of pharmaceutical formulation.
KEYWORDS: Method development; Validation; Derivative Spectroscopy; Piroxicam.
Piroxicam (Fig-1) is chemically (3E)-3-[Hydroxy-(pyridin-2ylamino)methylidene] -2-methyl-1,1- dioxobenzo[e]thiazin-4-one1. It has a potent anti-inflammatory action resulting from the reversible inhibition of cyclooxygenase-1, which ultimately results into the peripheral inhibition of prostaglandin synthesis.2 It is official in Indian Pharmacopoeia, British Pharmacopoeia and United States Pharmacopoeia.3-5. To the best of our knowledge, there is no report of UV-Visible spectrophotometric method for its estimation. Therefore, an attempt was made to develop a simple spectrophotometric method for the estimation of the present drug in formulations i.e. tablets.
Figure 1- Chemical structure of Piroxicam
EXPERIMENTALSECTION:
Instruments:
Analysis carried out on Lab India UV-3200 UV-VIS spectrophotometer, a double beam high speed scanning spectrophotometer (200-800 nm) with a photomultiplier tube detector and having variable spectral bandwidth (0.5-5.0 nm).
Chemicals and reagents:
Piroxicam was received as gratis sample by Shreeji Pharma International, Vadorada. All chemicals used were of analytical grade (E. Merck, India).
Standard stock solution:
To prepare stock solution of Piroxicam (PRC) (1000 μg/ml), 100 mg of PRC was placed in 100 ml volumetric flask and dissolved in 75 ml of Methanol and the volume was made up to the mark with Methanol. 10 ml of the solution was diluted up to 100 ml with methanol to produce final stock solution of 100 μg/ml of PRC.
Precision:
Twenty tablets (Mobicam-DT) were taken, powdered and powder weight equivalent to 20 mg of PRC was accurately taken and transferred to a 50 ml of volumetric flask. Twenty ml of methanol added to the same and sonicated for 30 min. The flask was shaken, and the volume was diluted to the mark with the same mixture. The above solution was filtered using whatman filter paper no. 1. Appropriate volume of the aliquot was transferred to a 50 ml volumetric flask and the volume was made up to the mark with methanol. The spectra were recorded and then measured at 335 nm for PRC.
Accuracy:
100 μg/ml concentrations of both standard stock solution and sample stock solution were prepared. To access the accuracy of the method, recovery experiment was performed at three different levels i.e. 80%, 100% and 120%. To the pre-analyzed sample solution a known amount standard drug solution was added at three different levels and absorbance were recorded. The % recovery was then calculated by using formula; 6,7,8 % Recovery = [A - B/ C] X 100, Where,
A = Total amount of drug estimated
B = Amount of drug found on preanalysed basis
C = Amount of Pure drug added.
The results recovery studies are reported in Table 2
RESULTS AND DISCUSSIONS:
The UV scan of standard solution between 200–400nm gives the absorption maxima at 335nm, shown in fig. 2.
Figure 2- Overlain spectra of Piroxicam
The Beer’s law was verified from the calibration curve by plotting a graph of concentration vs. absorbance. The plot is shown in fig. 3.
Figure 3- Calibration curve for Piroxicam
Table:1- Result of Precision
|
Sample |
Absorbance |
Amount Found (μg/ml) |
% Found |
|
Standard |
0.664 |
5 |
100 |
|
Sample-1 |
0.667 |
5.01 |
100.31 |
|
Sample-2 |
0.662 |
4.99 |
99.99 |
|
Sample-3 |
0.668 |
5.02 |
100.65 |
|
Sample-4 |
0.663 |
4.99 |
99.99 |
|
Sample-5 |
0.665 |
5.01 |
100.31 |
|
Sample-6 |
0.661 |
4.98 |
99.98 |
|
AVG |
0.664 |
5 |
100.20 |
|
SD |
0.0028 |
0.0154 |
0.269 |
|
RSD |
0.342 |
0.32 |
0.26 |
The UV scan of standard solution between 200 – 400 nm showed the absorption maxima at 335nm, shown in fig. 2. The Beer’s law was verified from the calibration curve by plotting a observed between 2-12 μg/ml. The plot clearly showed a straight line (0.1019X+0.1264) with the coefficient of correlation 0.999. The molar absorptivity was estimated as 127.6 g/100ml. The assay method was validated by low values of % RSD, indicating accuracy and precision of the methods as shown in Table 1 and Table 2. The percentage recovery of 99.78-100.5 proves the accuracy of the method.
Table 2: Result of Accuracy
|
|
Abs. |
Corr. Abs. |
ppm Added |
ppm Found |
% Recovery |
Mean |
|
80%-1 |
1.145 |
0.513 |
4 |
3.99 |
99.75 |
100.25 |
|
80%-2 |
1.142 |
0.515 |
4 |
4.01 |
100.25 |
|
|
80%-3 |
1.147 |
0.512 |
4 |
4.03 |
100.75 |
|
|
100%-1 |
1.274 |
0.632 |
5 |
5.02 |
100.4 |
99.93 |
|
100%-2 |
1.271 |
0.635 |
5 |
4.99 |
99.8 |
|
|
100%-3 |
1.276 |
0.631 |
5 |
4.98 |
99.6 |
|
|
120%-1 |
1.345 |
0.742 |
6 |
6.03 |
100.5 |
100.14 |
|
120%-2 |
1.347 |
0.746 |
6 |
5.99 |
99.83 |
|
|
120%-3 |
1.342 |
0.741 |
6 |
6.01 |
100.1 |
CONCLUSION:
From the results and discussion the method described in this paper for the determination of Piroxicam from tablet formulation is simple, accurate, precise and reproducible. The proposed method utilizes inexpensive solvents. The proposed method could be applied for routine analysis in quality control laboratories.
REFERENCES:
1. O'Neil, Maryadele J. et al The Merck Index, 14, 1294, 2006
2. http://www.drugbank.ca/drugs/DB00554/Piroxicam
3. Indian Pharmacopoeia Government of India Ministry of Health and Family Welfare 03, 1565, 2007.
4. British Pharmacopoeia, Medicines and Healthcare Products Regulatory Agency, 2, 1268 1269, 2007.
5. United States Pharmacopoeia – National Formulary, 28th edition, 2960, 2005.
6. ICH-Q2 (R1) Validation of Analytical Procedures: Methodology International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use, Geneva, Switzerland, 1996.
7. B.S. Nagaralli, J. Seetharamappa and M.B. Melwanki, J. Pharm. Biomed. Anal. 2002, 29, pp. 859–864.
8. C.C. Chan et. al., Analytical Method Validation and Instrument Performance Verification, Wiley Interscience, 2004, 67-84.
Received on 01.02.2016 Modified on 17.02.2016
Accepted on 28.02.2016 © AJRC All right reserved
Asian J. Research Chem. 9(2): Feb., 2016; Page 82-84
DOI: 10.5958/0974-4150.2016.00015.8