Author(s): Atul A. Shirkhedkar*, Ganesh S. Raut and Sanjay J. Surana
Department of Pharmaceutical Chemistry,
R. C. Patel Institute of Pharmaceutical Education and Research, Karwand Naka, Shirpur
Dist. Dhule 425 405 (M. S.) India
Email: atulshirkhedkar@rediffmail.com
Address for Correspondence
Dr. Atul A. Shirkhedkar*
Professor
Department of Pharmaceutical Chemistry,
R. C. Patel Institute of Pharmaceutical Education and Research, Karwand Naka, Shirpur
Dist. Dhule 425 405 (M. S.) India
Email: atulshirkhedkar@rediffmail.com
1

ABSTRACT
Lornoxicam (LOR) is used as non-steroidal anti-inflammatory drug. Two simple, precise and economical UV- Spectrophotometric methods have been established for the quantification of Lornoxicam in tablets. In Method I, Area Under Curve (AUC) was included in the wavelength range of 252 - 268 nm. Whereas, in Method II, zero order spectrum of Lornoxicam was deterivatized into first order (Δ λ = 4) using UV-probe software and AUC was integrated in wavelength range of 259 - 271.50 nm. In Method I and Method II, LOR obeyed linearity in the concentration range of 10 - 60 µg/mL and
20 - 100 µg/mL, respectively with r
2
> 0.999. Calibration curves were plotted using instrument response b e t w e e n p articular wavelengths and concentrations of analyte in the solution. The proposed methods were successfully applied for the determination of
LOR in commercial tablets and % amounts of LOR estimated by method I and method
II were found to be 99.09 % and 98.91 %, respectively. The proposed methods were validated as per ICH guidelines.
Key words: Lornoxicam , Spectrophotometric methods, Area under Curve, Tablets
2

INTRODUCTION
Lornoxicam (LOR) 6-chloro-4-hydroxy-2-methyl-N-2-pyridinyl-2H-thieno [2,3e ]-1,2thiazine-3-carboxamide 1,1-dioxide belongs to oxicam class of non-steroidal antiinflammatory(NSAID)
[1]
.
Literature survey revealed that L O R is estimated by HPLC [2 - 5] , HPTLC [6] and UV-
Spectrophotometric [7] and polarographic [8] methods in bulk material and pharmaceutical formulations
.
The present research paper deals with the development of zero order UV-
Spectrophotometric and first order Derivative UV-Spectrophotometric method using AUC technique for LOR in bulk and in tablets and to validate the methods as per ICH guidelines
[9, 10].
EXPERIMENTAL WORK
Material and Method
Lornoxicam working standard was obtained as gift from GLAXO SMITH KLINE, India
Spectroscopic grade NaOH purchased from LOBA Chemie Pvt. Ltd., Mumbai and double distilled water was used through the study. Analytical grade solution was used for the experiment.
Instruments
UV-Visible double beam spectrophotometer (UV-2450, SHIMADZU Limited, Japan) with1cm matched quartz cells and electronic balance (Model Shimadzu AUX 120)
Preparation of Stock Standard Solution and preparation of calibration curve
Stock standard solution was prepared by dissolving 10 mg of LOR in 0.1 N NaOH solutions to obtain concentration of 100 µg/mL
Method I: Zero Order UV-Spectrophotometric method using AUC technique
Aliquots of stock solutions were further diluted to get the concentrations in the range of 10 –
60 µg/mL of LOR and scanned in the range of 600 nm –200 nm. Zero order spectrum of
LOR obtained and two wavelengths 252- 268 nm were integrated for calculating AUC.
Method II: First Order Derivative UV-Spectrophotometric method Using AUC technique
Stock solutions was further diluted to obtain the concentrations in the range of 20 – 100
µg/mL and scanned in the range of 600 nm –200 nm. The zero order spectra of LOR were derivatized into first order ((Δ λ = 4, scaling factor = 8) and the two wavelengths
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259 – 271.50 nm were selected for determination of AUC.
The linearity curves were plotted in both these methods using instrument responses and concentrations obtained. The optical characteristics of LOR in both these methods are presented in table 1.
Analysis of tablet formulation
To estimate LOR in tablet formulation; twenty tablets were accurately weighed, average weight determined and ground into fine powdered. A quantity of powdered drug equivalent to 10 mg of LOR was transferred to 100 ml volumetric flask containing 40 ml of 0.1N NaOH , shaken manually for 15 min; volume was adjusted to mark with same solvent and filtered through Whatmann filter paper No.41. Resulting solution ( 40 µg /mL) was further diluted with same solvent and scanned and as mentioned in method I and II. The concentration of LOR determined in method I and II using respective linearity curves.
Accuracy of the methods
The accuracy of the proposed methods was studied by calculating mean % recovery performed at three different levels i.e. 80 %, 100% and 120 %. To the pre-analyzed sample solution a known amount of LOR bulk drug was added at 80 % to 120 % and the re-analyzed the LOR by proposed methods, the results are shown in table 2.
RESULTS AND DISCUSSION
For dissolving LOR 0.1 N NaOH was chosen as solvent. In method I and II, LOR followed linearity in the concentration range of 10 – 60 µg/ mL and 20 -100 µg/ mL, respectively. The details of optical characteristics are given in table 1.
The % amount of LOR estimated by method I and II was found to be 99.09 % and 98.91%, respectively. Results indicated that there was no interference from the excipients generally occurs in tablet formulation.
The developed methods were validated for accuracy, precision and ruggedness as per ICH guidelines.
The accuracy methods were studied as mean % recovery and found to be in the range of
98.93 - 101.08 (method I) and 99.30 -100.45 (method II), respectively.
The precision of the methods was determined as repeatability, intra-day and inter-day study.
An appropriate concentration 20 μg/mL, 30 μg/mL and 50 μg/mL in method I and 30 μg/mL,
50 μg/mL and 80 μg/mL ( method II) were selected and instrumental response were determined.
Ruggedness of the proposed methods was determined by analyzing aliquots from homogenous slot 30 μg/mL (method I) and 40 μg/mL (method II) by different analyst using
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similar operational and environmental conditions. The results are reported in terms of %
RSD. The results from validation of methods are shown in table 3.
CONCLUSION
Both these developed UV-Spectrophotometric methods are simple, accurate and precise and be used for routine analysis of LOR from its tablet formulation.
REFERENCES
1.
Budavari S. The Merck Index.
12 th ed. New Jersey, USA, Merck and Co. Inc. (1996) 6420
2.
Attimarad M., Rapid RP-HPLC method for quantitative determination of Lornoxicam in tablets, Journal of Biological and Clinical Pharmacy 2010, 1(2), 115-118.
3.
Patil K., Rane V., Sangshetti J., Shinde D. LC method for analysis of Lornoxicam in the dosage form, Journal of Chromatographia 2009, 69(9-10), 1001-1005.
4.
Zhang JJ, Gao Y, Fan WM, Ren BJ. Development and Validation of HPLC method for the estimation of Lornoxicam in Pharmaceutical formulation, Journal of American
Association of Pharmaceutical Scientists 2004, 63, 285-290.
5.
Bhavsar SM., Patel DM., Khandhar AP., Patel CN. Validated RP-HPLC method for simultaneous estimation of Lornoxicam and Thiocolchicoside in solid dosage form,
Journal of Chemical Pharmaceutical Research 2010, 2(2), 563-572.
6.
Hable AA, Raut RP, Chaudhari VP. Development and validation of a HPTLC method for simultaneous estimation of lornoxicam and thiocolchicoside in combined dosage form pharmaceutical methods 2011, 2(3), 178-183.
7.
Nemutlu E, Demircan S, Kir S. Determination of Lornoxicam in Pharmaceutical
Preparation by Zero and First order derivative UV Spectrophotometric methods,
Pharmazie 2005, 60(6), 421-425.
8.
Cetin I, Kocak N, Aycan S. Polarographic determination of Lornoxicam in
Pharmaceutical Formulations, C.B.U. Journal of Science 2009, 5(1), 11-18.
9.
ICH guidelines Q2A. In; Text on Validation of analytical procedures, International
Conference on harmonization, Geneva 1994.
10.
ICH guidelines Q2B. In; Validation of analytical Procedures; Methodology. International conference on harmonization, Geneva 1996.
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Tables and Captions
Table 1; Optical characteristics of Lornoxicam
Table 2; Accuracy
Table 3; Ruggedness
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Table: 1 Optical characteristics of Lornoxicam
Parameters
Beer-Lambert’s range(μg/mL)
λ max(nm)/ wave length range (nm)
Regression Equation
Slope
Intercept
Correlation coefficient (r
2
)
Limit of detection (μg/mL)
Limit of quantitation (μg/mL)
Method I
10 - 60
252-268
0.029X+ 0.010
0.029
0.10
0.999
0.89
2.66
Method II
20-100
259- 271.50
0.032X - 0.103
0.032
0.103
0.999
1.64
5.81
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Table 2: Accuracy
Method
I
Method
II
Initial amount
(μg/mL)
20
20
20
40
40
40
%
Amount of drug
Added
Method I
% Recovery % RSD
80
100
120
98.93
99.87
101.08
0.52
0.40
0.74
99.30
100.37
100.45
Method II
% Recovery % RSD
0.34
0.30
0.22
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Table 3: Ruggedness
Analyst 1
[%RSD]
Method I Method II
1.03 1.10
Analyst 2
[%RSD]
Method I
0.80
Method II
1.53
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Figure No.1: Zero order AUC spectrum of Lornoxicam in NaOH
Figure No.2: First order AUC spectrum of Lornoxicam in NaOH
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Figure 1: Zero order AUC spectrum of Lornoxicam in NaOH
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Figure 2: First order AUC spectrum of Lornoxicam in NaOH
12