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ORIGINAL ARTICLE
Year : 2010  |  Volume : 2  |  Issue : 2  |  Page : 121-123 Table of Contents     

Spectrophotometric estimation of betahistine hydrochloride in tablet formulations


1 Department of Pharmaceutical Analysis, Swami Keshvanand Institute of Pharmacy, Bikaner, Rajasthan, India
2 Department of Pharmaceutics, Maharishi Dyanand University, Rohtak, Haryana, India

Date of Submission19-Mar-2010
Date of Decision07-Apr-2010
Date of Acceptance22-May-2010
Date of Web Publication2-Aug-2010

Correspondence Address:
Amit Kumar
Department of Pharmaceutical Analysis, Swami Keshvanand Institute of Pharmacy, Bikaner, Rajasthan
India
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Source of Support: None, Conflict of Interest: None


DOI: 10.4103/0975-7406.67013

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   Abstract 

Aim: The study aims to develop simple, sensitive, rapid, accurate and precise spectrophotometric method for estimation of Betahistine hydrochloride in tablet dosage forms. Materials and Methods: For method I and II, in a series of 10 ml volumetric flask, aliquots of standard drug solution (100 μg/ml) in double distilled water were transferred and diluted with same so as to give several dilutions in concentration range of 15-90 μg/ml and 10-80 μg/ml respectively of betahistine hydrochloride. To 5 ml of each dilution taken in a separating funnel, (5 ml of methyl orange for method I and 5 ml of bromo phenol blue for method II) reagent and 5 ml of chloroform was added. Reaction mixture was shaken gently for 5 min and allowed to stand so as to separate aqueous and chloroform layer. Absorbance maxima measured at 421.6 nm and 412 nm for method I and II respectively. Results: The recovery studies were found close to 100 % that indicates accuracy and precision of the proposed methods. The statistical analysis was carried out and results of which were found satisfactory. Standard deviation values were found low that indicated reproducibility of the proposed methods. Conclusion: Based on results the developed methods could be used for routine estimation of betahistine hydrochloride from tablet formulations.

Keywords: Betahistine hydrochloride, bromo phenol blue, methyl orange, spectrophotometric estimation


How to cite this article:
Kumar A, Nanda S, Chomwal R. Spectrophotometric estimation of betahistine hydrochloride in tablet formulations. J Pharm Bioall Sci 2010;2:121-3

How to cite this URL:
Kumar A, Nanda S, Chomwal R. Spectrophotometric estimation of betahistine hydrochloride in tablet formulations. J Pharm Bioall Sci [serial online] 2010 [cited 2020 Feb 22];2:121-3. Available from: http://www.jpbsonline.org/text.asp?2010/2/2/121/67013

Betahistine hydrochloride is an orally administered anti-histaminic drug. The chemical name of Betahistine is N-methyl-2-(pyridin-2-yl)-ethanamine. Betahistine has a very strong affinity for histamine H 3 receptors and a weak affinity for histamine H 1 receptors. It has been used to control vertigo in patients of Meniere's disease; it possibly acts by causing vasodilation in the internal ear. [1],[2] Several methods have been reported for the estimation of betahistine hydrochloride. The British pharmacopoeia and Merck Index describe thin layer chromatography and the liquid chromatography method for assay of betahistine hydrochloride. [3],[4] A literature survey reveals one HPLC [5] and one liquid chromatographic method [6] for the determination of betahistine hydrochloride in pharmaceutical preparations. To the best of our knowledge, prior to our study, there has been no reported spectrophotometric method for the determination of betahistine hydrochloride in pharmaceutical formulations. Thus, efforts are being made to develop a fast, selective, and sensitive analytical method for the estimation of betahistine hydrochloride in its tablet formulations.


   Materials and Methods Top


Materials

Shimadzu UV 1700, UV-Visible double beam spectrophotometer with spectral band width of 1 nm, wavelength accuracy of ± 0.3 nm, and 1.0 cm matched quartz cells were used for analytical method development. All the chemicals and reagents used were of analytical grade. Betahistine hydrochloride (99.55% pure), generously supplied by Albert David Ltd., (Kolkata, India), was used as such, without further purification. Methyl orange and Bromo phenol blue (Loba Chemie, Mumbai) reagents were prepared in double distilled water. All the reagents were extracted several times with chloroform so as to remove the chloroform-soluble impurities. Tablet formulations of betahistine hydrochloride were procured from a local pharmacy. Betavert tablet 8 mg, Sun Pharmaceutical Pvt. Ltd. and Verbet-8 tablet 8 mg, Albert David Ltd., were procured from the local market. A standard solution of betahistine hydrochloride was prepared by dissolving 10 mg in 100 ml of double distilled water to give a stock solution of concentration 100 μg/ml of the drug.

Methods

Procedure for preparation of calibration curve

For method I, in a series of 10 ml volumetric flasks, aliquots of the standard drug solution (100 μg/ml) in double distilled water were transferred and diluted with the same, so as to give several dilutions in the concentration range of 15 - 90 μg/ml of betahistine hydrochloride. To 5 ml of each dilution taken in a separating funnel, 5 ml of methyl orange (0.5% w/v) reagent and 5 ml of chloroform were added. The reaction mixture was shaken gently for five minutes and allowed to stand, so as to separate the aqueous and chloroform layers. The chloroform layer was separated out and an absorbance maximum was measured against a reagent blank. The calibration curve was plotted [Figure 1] between the concentrations of betahistine hydrochloride and the measured absorbance.

For method II, in a series of 10 ml volumetric flasks, aliquots of the standard drug solution (100 μg /ml) in double distilled water were transferred and diluted with the same, so as to give several dilutions in concentration range of 10 - 80 μg/ml of betahistine hydrochloride. To 5 ml of each dilution taken in a separating funnel, 5 ml of bromo phenol blue reagent (0.5% w/v) and 5 ml of chloroform were added. The reaction mixture was shaken gently for five minutes and allowed to stand, so as to separate the aqueous and chloroform layers. The chloroform layer was separated out and an absorbance maximum was measured against a reagent blank. The calibration curve was plotted [Figure 2] between the concentrations of betahistine hydrochloride and measured absorbance. The spectral characteristics of betahistine hydrochloride for method I and method II are given in [Table 1].

Method validation

Calibration curve (linearity of the method)

The calibration curves were constructed by plotting absorbance versus concentrations of betahistine, after which the regression equations were calculated. The calibration curves were plotted over six different concentrations in the range of 15 - 90 μg/ml for method I and 10 - 80 μg/ml for method II.

Accuracy (% Recovery)

The accuracy of the methods was determined by calculating the recoveries of betahistine by the standard addition method. Known amounts of mixed standard solution of betahistine were added to prequantified sample solutions of the tablet dosage forms. The amounts of betahistine were estimated by applying values of absorbance to the regression equations of the calibration curve and the results of the recovery studies are reported in [Table 2].

Method precision (Repeatability)

The precision was checked by repeatedly scanning (n = 6) the standard solutions of betahistine hydrochloride (10 μg/ml), and the low value of standard deviation as well as relative standard deviation showed good method precision.

Intermediate precision (Reproducibility)

The intermediate precision for the proposed method was determined by estimating a standard solution of betahistine hydrochloride for three different concentrations, thrice. The results are reported in terms of relative standard deviation (RSD).

Specificity

The excipients, gelatin, hypromellose, hydroxypropyl methylcellulose acetate succinate, sodium lauryl sulfate, sucrose, talc, titanium dioxide, and triethyl citrate (Signet Ltd., Mumbai, India) were spiked into a preweighed quantity of drugs, to assess the specificity of the methods. The absorbance was measured to determine the quantity of the drugs.

Robustness

Solutions of the drug were studied for their stability at an ambient temperature for 24 hours. The results were unaffected by the small, but deliberate variations in the method parameters, and provided an indication of its reliability during normal usage. [7]

Procedure for analysis of tablet formulation

For analysis of tablet formulation 20 tablets (8 mg) of betahistine hydrochloride were weighed accurately and finely powdered. An accurately weighed, powdered sample, equivalent to 10 mg of betahistine hydrochloride, was taken in a 100 ml volumetric flask containing 40 ml of double distilled water, and sonicated for 10 minutes. The resultant was filtered through Whatman filter paper No. 41 into another 100 ml volumetric flask. The filter paper was washed several times with double distilled water. The washings were added to the filtrate and the final volume was brought up to the mark with double distilled water.

For method I, 4.5 ml of filtrate from the sample solution was diluted to 10 ml with double distilled water. This was treated as per the procedure used in the preparation of the calibration curve and the amount of drug present in the sample was computed from the respective calibration curve.

For method II, 4.0 ml of filtrate from the sample solution was diluted to 10 ml with double distilled water. This was treated as per the procedure used in the preparation of the calibration curve and the amount of drug present in sample was computed from the respective calibration curve. The procedure of analysis from tablet formulations for all the methods were repeated five times with two different tablet formulations and the results are reported in [Table 2].

Recovery studies

Recovery studies were carried out for both the developed methods by addition of a known amount of standard drug solution of betahistine hydrochloride to a pre-analyzed tablet sample solution at three different concentration levels. The resulting solutions were analyzed by the proposed methods. The results of the recovery studies are reported in [Table 2].


   Result and Discussion Top


The development of a new dosage form involves a number of stages and the analytical methods that are specific, accurate, and precise, play a vital role in many of the essential features required for an identical analytical system, and have been adopted in a wide range of pharmaceutical analysis. Taking into account the above-mentioned characteristics, two accurate, simple, precise, economical, and rapid visible spectrophotometric assay methods were developed, for the quantitative estimation of betahistine hydrochloride in tablet dosage forms.

The optimum reaction conditions for the quantitative determination of ion pair complexes were established via a number of preliminary experiments. To test the accuracy and reproducibility of the proposed methods, the recovery experiments were carried out by adding a known amount of drug to the pre-analyzed formulation and reanalyzing the mixture using the proposed methods.

Stability studies of chromogen were carried out by measuring the absorbance values at a time interval of 10 minutes, for 4 hours, and it was found to be 30 minutes for both methods. The optical characteristics such as absorption maxima, Beer's law limits, correlation coefficient (r), slope (m), y-intercept (c), and molar absorptivity calculated from nine replicate readings are incorporated in [Table 1]. The analysis results of the marketed formulations are in good agreement with the official methods. The reproducibility, repeatability, and accuracy of these methods were found to be good, which is evident by the low standard deviation values (0.308 for method I and 0.385 for II). The percentage of recovery values obtained were 99.50 for I and 99.34 for II, which indicated no interference from the excipients used in the formulation. Hence, these developed methods could be used for the routine estimation of betahistine hydrochloride in tablet formulations. The results are shown in [Table 2].

 
   References Top

1.Tripathi KD. Autacoids and related drugs: Essential of medical pharmacology. 5 th ed. New Delhi: Jaypee brothers medical publishers; 2006. p.138.  Back to cited text no. 1      
2.Sharma VN. Autacoids and their antagonists: Essential of pharmacology. 2 nd ed. New Delhi: CBS Publishers and distributors; 2005. p. 542.  Back to cited text no. 2      
3.Budavari S, editor. The Merck Index. 14 th ed. Whitehouse Station, NJ: Merck and Co Inc;1996. p. 1178.  Back to cited text no. 3      
4.British Pharmacopoeia. Vol. 3. United Kingdom: The Stationary office on the behalf of MHRA; 2009. p. 245.  Back to cited text no. 4      
5.EI Wality AF, Razak OA, Belal SF, Bakry RS. Utilization of carbon disulphide for the analytical determination of betahistine hydrochloride and captopril in their pharmaceutical preparation. J Pharm Biomed Anal 1999;21:439-49.  Back to cited text no. 5      
6.Douglas JF, Hohing TL. GLC determination of betahistine in serum. Experientia 1978;34:499-500.  Back to cited text no. 6      
7.CPMP/ICH/281/95, Note for Guidance on Validation of Analytical Procedures: Methodology, ICH Topic Q2B Validation of Analytical Procedures: Methodology, Step 4 (CPMP Adopted Dec 96).  Back to cited text no. 7      


    Figures

  [Figure 1], [Figure 2]
 
 
    Tables

  [Table 1], [Table 2]


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[Pubmed] | [DOI]



 

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