Development and Validation of UV Spectrophotometric method for estimation of Lafutidine in bulk and Pharmaceutical dosage form

Parekh Ravishkumar R*, Patel Pinkal H, Patel Chinmay D, Patel Krupali S, Patel Hardik N
Department of pharmaceutical Quality Assurance, Baroda college of Pharmacy, Parul Trust, Gujarat Technological University, Limda-391760, Vadodara, Gujarat, India.
Corresponding Author: Parekh Ravishkumar. R., Quality Assurance laboratory, Department of pharmaceutical Quality Assurance, Baroda college of Pharmacy, Parul Trust, Limda-391760, Vadodara, Gujarat, India. Email: [email protected] Phone: 09427548613
Received:02 March 2012 Accepted: 09 March 2012
Citation: Parekh Ravishkumar R*, Patel Pinkal H, Patel Chinmay D, Patel Krupali S, Patel Hardik N “Development and Validation of UV Spectrophotometric method for estimation of Lafutidine in bulk and Pharmaceutical dosage form”, Int. J. Drug Dev. & Res., Jan-March 2012, 4(1): 325- 329 doi: doi number
Copyright: © 2010 IJDDR, Parekh Ravishkumar et al. This is an open access paper distributed under the copyright agreement with Serials Publication, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.
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Abstract

A simple, rapid, accurate, precise, sensitive and economical UVspectrophotometric method has been developed for estimation of Lafutidine from bulk and pharmaceutical formulation. The max of Lafutidine in 0.1N HCL was found to be 286 nm. The parameters linearity, precision, accuracy, limit of detection and limit of quantitation, ruggedness were studied according to International Conference on Harmonization guidelines. The drug follows linearity in the concentration range 5- 50μg/ml with correlation coefficient value 0.9995. The proposed method was applied to pharmaceutical formulation and % amount of drug estimated 99.19 % was found in good agreement with the label claim. The accuracy of the method was checked by recovery experiment performed at three different levels i.e., 80%, 100% and 120 %. The % recovery was found to be in the range 99.57%– 99.91%. The low values of % R.S.D. are indicative of the accuracy and reproducibility of the method. The precision of the method was studied as an intra-day, inter-day variations and repeatability. The % R.S.D. value less than 2 indicate that the method is precise. The above method was a cost-effective quality- control tool for routine analysis of Lafutidine in bulk and in pharmaceutical dosage form.

Keywords

Lafutidine, Anti Ulcer, UV, Quantitative determination, 0.1 N HCl.

INTRODUCTION

Lafutidine is chemically 2-(furan-2-ylmethylsulfinyl)- N-[4-[4-(piperidin-1-ylmethyl)pyridin-2-yl]oxybut-2- enyl]acetamide. Lafutidine is not official in any pharmacopoeias.
Lafutidine is the new generation H2-receptor antagonist. It blocks the production of acid by acidproducing cells in the stomach and blocks histamine H2-receptors in the stomach and prevents histaminemediated gastric acid secretion. It is indicated in hyperacidity, NSAID induced gastritis, gastric and duodenal ulcers and also used as preanesthetic medication. Apart from H2-receptor blockade activity, it has additional gastro protective action. Therefore not only inhibit acid secretion but also provide gastric mucosal protection.
The literature survey revealed that various methods of analysis for Lafutidine have been reported, which included, LC-ESI-MS[5,6] ,HPLC-MS[7],LC Tandem MS[8] .There is no reported spectrophotometric methods. Thus efforts are made to develop a simple, accurate, precise method for estimation of Lafutidine in bulk and solid dosage form using simple UV spectrophotometric method.

EXPRIMENTAL

Chemical and reagents
0.1N HCl was used throughout UV spectrophotometric method development and validation.
Instrumentation
UV spectrophotometric method was performed on double beam UV-visible spectrophotometer (Shimadzu, model 1800) having two matched quartz cells with 1 cm light path
Preparation of standard stock solution (100μg/ml)
Accurately weighed quantity of 100 mg Lafutidine was transferred to 100 ml volumetric flask and dissolved in 25 ml of 0.1N HCl by shaking manually for 2 minutes. The volume was made up with the same up to the mark to give concentration of 1000μg/ml. From this pipette out 10 ml of solution in another 100 ml volumetric flask and volume was made up with the 0.1N HCl up to the mark to give final concentration of 100μg/ml.
Preparation of sample stock solution (100μg/ml)
To measure the Lafutidine content of tablet (label claim 10 mg Lafutidine per tablet, Laciloc tablet by Cadila Pharmaceuticals, Dholka, Ahmedabad), twenty tablets were weighed, the mean weight was determined. A weight of the powder equivalent to10 mg Lafutidine was transferred to a 100 ml volumetric flask containing 50 ml 0.1N HCl and the mixture was sonicated for 20 min then made up to 100 ml with 0.1N HCl gives concentration of 100μg/ml. The solution was filtered and filtered solution was used throughout experiment.
Validation of UV spectrophotometric method:
The method was validated in terms of linearity, accuracy, precision, ruggedness, sensitivity.
Linearity study:
Different aliquots of Lafutidine from standard stock solution in the range of 0.5–5.0 ml were transferred into series of 10 ml volumetric flask and volume made up to the mark with 0.1N HCl to get concentration of 5–50μg/ml, respectively. The solutions were scanned on spectrophotometer in the range of 200 – 400 nm. The spectrum was recorded at 286 nm. The calibration curve of absorbance vs. concentration was plotted and correlation co-efficient and regression line equation for Lafutidine were determined.
Precision:
Precision of the method was studied as intra-day and inter-day variations. Intra-day precision was determined by analyzing 10, 25 and 40μg/ml of Lafutidine solutions for three times in the same day. Inter-day precision was determined by analyzing 10, 25 and 40μg/ml of Lafutidine solutions daily for three days in the week.
Repeatability
Repeatability was determined by analyzing 25μg/ml concentration of Lafutidine solution for six times within short interval of time.
Accuracy: (Recovery)
Accuracy was determined by performing recovery studies by spiking different concentration of pure drug in pre-analyzed sample solution. To preanalyzed sample solution, a known amount of standard stock solution was added at different level i.e. 80%, 100% and 120%. The solutions were reanalyzed by proposed method
Sensitivity:
The sensitivity of measurements of Lafutidine by the use of the proposed method was estimated in terms of the Limit of Quanfication (LOQ) and Limit of Detection (LOD). The LOD and LOQ were calculated using formula LOD= 3.3*M/S and LOQ= 10*M/S Where, M = the standard deviation of y-intercepts of regression lines, S = the slope of the calibration curve.
Ruggedness:
The solutions were prepared and then analyzed with change in the analytical condition like different laboratory, different analyst, different instrument.
Determination of Lafutidine in bulk:
Accurately weighed 10 mg of Lafutidine was transferred into 100 ml volumetric flask containing 20 ml 0.1N HCL and volume was made up to the mark using 0.1N HCl. Appropriate volume 3 ml of this solution was transferred to 10 ml volumetric flask and volume was made up to mark using 0.1N HCl to give concentration of 30μg/ml. The resulting solution was scanned on spectrophotometer in the UV range 200 - 400 nm. The concentrations of the drug were calculated from linear regression equations.
Analysis of pharmaceutical formulation by proposed UV spectrometric method:
From the sample stock solution, 3 ml of the solution was taken in 10 ml volumetric flask and made up to mark with 0.1N HCL to give concentration of 30μg/ml. The resulting solution was scanned on spectrophotometer in the UV range 200 - 400 nm. The concentrations of the drug were calculated from linear regression equations.

RESULTS AND DISCUSSION

Method Validation
The proposed method was validated as per ICH guideline Q2 (R1).
Linearity studies:
The linearity of Lafutidine was found to be in the range of 5–50μg/ml with correlation coefficient of 0.9995. Linear regression equation was found to be Y = 0.0166X – 0.0082. The calibration data is expressed in Table 1, calibration curve is shown in Figure 2 and overlay spectra in Figure 3.
Precision:
The precision of the method was expressed in terms of % relative standard deviation (%RSD). The %RSD values found to be less than 2 for intra-day and interday precision, which indicate that the proposed method is precise for analysis. The result is expressed in Table 2 and Table 3.
Repeatability:
Repeatability was determined by analyzing 25μg/ml concentration of Lafutidine solution for six times and %RSD was found to be 0.72, which is less than 2. The results is expressed in Table 4.
Accuracy (Recovery):
Accuracy of the method was confirmed by recovery study from marketed formulation at three level of standard addition. %Recovery for Lafutidine was found to be 99.57-99.91%. The recovery studies are reported in Table 5.
Sensitivity:
The linearity equation was found to be Y = 0.0166X – 0.0082. The LOD and LOQ for Lafutidine were found to be 0.293μg/ml and 0.887μg/ml, respectively.
Ruggedness:
Absorbance was measured for same concentration solutions, six times. The results are given in Table 6.
Determination of Lafutidine in bulk:
The concentrations of the drug were calculated from linear regression equations. The % assay found was between 99.43% to100.43% as shown in Table 7.
Analysis of pharmaceutical formulation by proposed UV spectrophotometric method:
The concentrations of the drug were calculated from linear regression equations. The % assay found was between 98.63% to 99.63% as shown in Table 8.

CONCLUSION:

The proposed UV spectrophotometric method for the determination of Lafutidine in bulk and pharmaceutical dosage form was found to be simple, accurate, precise, rapid, sensitive and economical. Lafutidine shows maximum absorbance at 286 nm. The validation of the method conforms that this is an appropriate method for determination of Lafutidine in bulk and pharmaceutical dosage form. The proposed method can be used for routine quality control of bulk drug as well as formulations containing Lafutidine

Acknowledgement:

The authors are thankful to the Project guide Mrs. Pinkal Patel and management, Baroda college of Pharmacy, Limda, Gujarat for providing the all facilities to carry out this research work.

Conflict of Interest

NIL

Source of Support:

NONE

Tables at a glance

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Table 1 Table 2 Table 3 Table 4
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Table 5 Table 6 Table 7 Table 8
 

Figures at a glance

Figure 1 Figure 2 Figure 3
Figure 1 Figure 2 Figure 3
 

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