UV-Spectroscopic Estimation and Validation of Drotaverine Concentration in Bulk and Dosage Form

 

Vedantika Das¹*, Ashwini Sambherao¹, Saroj Gajare, Amar Zalte¹, Dr. R. B. Saudagar²

 

ABSTRACT:

A simple, accurate, precise, and sensitive a highly selective ultra violet spectrophotometric method has been developed for the validation and estimation in bulk and dosage form. It shows maximum absorbance 286 nm. Beer-Lambert’s was obeyed in the concentration range of in the range of 15-55µg/ml. The method was successfully validated in accordance to ICH guideline for accuracy, precision, linearity and robustness. The linear regression analysis data for calibration plots showed good linear relationship and obtain correlation factor 0.9927 for Drotaverine. Thus method was successfully applied for routine analysis of Drotaverine in bulk samples.

 

 

 

INTRODUCTION:

Drotaverine hydrochloride (DRO) Chemically 1-[(3, 4-[diethoxyphenyl) methylene]-6,7-Diethoxy-1,2,3,4-tetra hydroisoquinolene; 1-(3,4-diethoxybenzylidene)-6,7diethoxy-, 2,3,4tetrahydroisoquinoloine; isodihydroperparine.C₂₄H₃₁NO₄ ; mol.wt-397.51.C 72.52%,H, N 3.52%, O 16.10%,  A papaver analogue mainly used as an antispasmodic and smooth-muscle relaxant in pain associated with gastrointestinal colic, biliary colic, and postsurgical spasms. Drotaverine has been shown to possess dose-dependent analgesic effects in animal model.

 

 

Figure-1 Drotaverine HCL

 

MATERIALS AND METHODS:

Chemical and Reagents:

Analytically pure Drotaverine were obtained as gift Walter-Bushnell. Commercial tablet formulations were purchased from the local market.  All chemicals and reagents used were of Analytical Grade, obtained from Merck.

 

Instrument:

A Jasco double beam UV/Visible spectrophotometer (Model: Jasco V-360) and Borosil glass wares were used for the study. Calibrated electronic single pan balances Shimadzu AY220, ultra-sonication were also used during the analysis.

Standard Stock Solution:

The standard stock solutions of Drotaverine hydrochloride was prepared by dissolving accurately weighed 10 mg drug in 100ml double distilled water.

 

Determination of λmax :

The standard solution of both Drotaverine Hydrochloride and API (10 μg/ml) were scanned in the wavelength region of 200-400nm and the λmax was found to be 286nm.

 

Preparation of calibration curve:

For each of drug, appropriate aliquots were pipette out from each standard stock solution into a series of 10 ml volumetric flasks. The volume was made up to mark with double distilled water to set of solutions having concentration range 10-100μg/ml for both Drotaverine  Hydrochloride and API five dilutions of each concentration of each drug were prepared separately. The prepared working solutions of Drotaverine Hydrochloride and API were scanned at 286nm.Therespective absorbance was recorded and absorbance was plotted against the concentrations to obtain their respective calibration curves.

Preparation of Sample Stock Solution:

Contents of two tablets were weighed accurately and powdered. Powder equivalent to 10mg of DRO was weighed and dissolved in 100 mL of water.

 

METHOD VALIDATION:

Validation is a process establishing documented evidence which provides a high degree of assurance that a specific activity will consistently produce a desired result or product meeting pre-determine specifications and quality characteristics. The method was validated for different parameters like linearity, accuracy, precision, robustness, ruggedness.    

 

Linearity:

Various aliquots were prepared form the stock solution ranging from 15-55µg/ml. The samples were scanned in UV-VIS spectrophotometer using distilled water as a blank. It was found that the selected drug shows linearity between range 15-55µg/ml.

 

 

 

Figure-2 Calibration Curve of Marketed DRO

 

 

Figure-3 Calibration Curve of API

 

 

Accuracy:

The accuracy of the method was determined by preparing solutions of different concentrations that is 80%, 100%&120% in which the amount of marketed formulation (10mg) was kept constant and the amount of pure drug was varied that is 8mg, 10mg & 12mg for 80%, 100%&120% respectively. The solutions were prepared in triplicates and the accuracy was indicated by % recovery.

 

Precision:

Precision of the method was demonstrated by intraday & interday variation studies. In intraday variation study, the data for DRO at 286nm the % R.S.D value was found to be ±indicated that the method is precise.

Interday precision

The data for interday precision for DRO is shown in table.  The % R.S.D value was found to be ±2 indicated that the method is precise.

 

Ruggedness:

The method was determined by analyzing same sample (different batches) by different analysts at different conditions and the respective absorbance were noted. 

 

Robustness:

The method was determined by carrying out the analysis at two different wavelengths i.e. at (±2 nm and -2nm)

 

RESULT AND DISCUSSION

TABLE 1: ACCURACY

Concentration	S.D	%R.S.D
20	0.02381	1.0582
25	0.00334	0.1611
30	0.001	0.0504

 

Table 2: PRECISION

Intra-day	S.D	% R.S.D
Inter- day	0.01805 0.02450	0.2889 0.3898

 

Table 3: Accuracy (API)

Concentration	S.D	% R.S.D
20	0.0026	0.1482
25	0.0504	1.9616
30	0.0244	1.4144

 

Table 4: Precision

Intra-day	S.D	%R.S.D
Inter-day	0.0194 0.0223	1.3211 1.4321

 

TABLE 5:Recovery data of Bulk drug and API

% Recovery (mean ±S.D)	% R.S.D
Bulk drug	1.133
API	1.145

 

 

CONCLUSION:

UV-Spectroscopic estimation and validation method was successfully developed for drotaverine hydrochloride in bulk and dosage form. The method for both bulk and dosage form at the selected wavelength was found to be accurate and precise as indicated by interday and intraday analysis, showing percent relative standard deviation (%R.S.D) is  within limit. Marketed tablets were analyzed and amount of drug was determined by proposed method is good agreement with the label claim. 

 

REFERENCE:

1.       Ziyatdinova K, Samigullin I, and Budnikov K (2007) Volta metric determination ofpapaverine and drotaverine. J. Anal. Chem. 62:773.

2.       El-Wasseef D, El-Sherbiny D, Eid M, and Belal F (2008) Spectrofluorometric determination of drotaverine hydrochloride in pharmaceutical preparations. Anal. Lett 41:2354

3.       Metwally F H (2008) Simultaneous determination of nifuroxazide and Dortaverine hydrochloride in pharmaceutical preparations by bivariate and multivariate spectra analysis Spectrochim. Acta A. 69:343.

4.       Abdellatef E, Ayad M, Soliman M and Youssef F (2007) Spectrophotometric and spectrodensitometric determination of paracetamol and drotaverine HCl in combination. Spectrochim. Acta A 66:1147.

5.       Panigrahi D and Sharma R (2008) Development and validation of an RP-HPLC method for simultaneous analysis of dortaverine and omeprazole in a tablet dosage form. Acta Chromatographica 20:439.

6.       Indian Pharmacopoeia (2007) the Indian Pharmacopoeia Commission: Ghaziabad, Volume IIand p 681.

7.       Oneil M J, Smith A and Heckelman P E (2001) The Merck Index, 13th edition Merck, Whitehouse Station: New Jersey, p 3489.

 

 

 

Received on 07.07.2016       Accepted on 01.08.2016     

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