Implementation UV-Spectrophotometry approach for Determination of Tamsulosin HCl in tablets using area under Curve Technique

 

Prajakta D. Mhaske1, Burhan A. Bohari2, Suraj R. Chaudhari1, Pritam S. Jain1, Atul A. Shirkhedkar1*

1Department of Pharmaceutical Chemistry, R. C. Patel Institute of Pharmaceutical Education and Research, Shirpur, (MS) 425405

2Department of Pharmaceutical Quality Assurance, R. C. Patel Institute of Pharmaceutical Education and Research, Shirpur, (MS) 425405

*Corresponding Author E-mail: shirkhedkar@gmail.com

 

ABSTRACT:

A validated sensitive and accurate zero-order area under curve spectrophotometric method was adopted for analysis of tamsulosin hydrochloride in pure form and pharmaceutical dosage form. The area of peak was measured in the wavelength range of 220-227.60 nm by dissolving pure drug and dilution was made in a mixture of methanol and water (30:70 %). Linearity plot was constructed and linearity was followed in the concentration range of 5-35 μg/mL with correlation coefficient (r2) 0.997. The developed method was successfully implemented for the determination of tamsulosin hydrochloride in pharmaceutical preparation and amount of analyte was estimated was found to be 98.53 ± 0.62 %. The results obtained indicate no interference from excipients present in pharmaceutical preparation. Moreover, the present work was validated statistically with respect to the accuracy, precision,the limit of detection and of quantification and ruggedness. The result of all parameters was analysed and indicated that the established method can be classified amongst highly sensitive and accurate procedure. Moreover, the established method was compared with the reported method. These merits suggested the use of the proposed method in routine and quality control analysis of tamsulosin hydrochloride without the interference of common excipients in a dosage form. Further, the established method is validated as per international conference on harmonization guidelines.

 

KEYWORDS: Tamsulosin hydrochloride; area under Curve; UV-Spectrophotometry; validation.

 

 

 

 

1.    INTRODUCTION:

Tamsulosin hydrochloride (TH) chemically is (R)-5-(2 {[2- (o-ethoxyphenoxy) ethyl] aminopropyl)-2-methoxybenzenesulfonamide hydrochloride shown in Figure 1. TH is a sulphonamide derivative with selective α1 adrenoreceptor antagonist. TH actually works in the human prostate and bladder neck. It specifically acts on and inhibits the action of α1adrenoreceptor in order to relax the smooth muscle in prostate and bladder neck resulting in increased urinary discharge amounts [1-3]. TH broadly metabolized in the liver by the cytochrome enzyme and the metabolites undergo largely conjugation to glucuronide or sulphate before to renal excretion [4, 5].

 

Figure 1: Chemical structure of Tamsulosin hydrochloride

 

The spectrophotometric methods are the most simple, economical technique and superior to the liquid chromatography techniques with respect to the simple instrumentation, speed of analysis and consumption of less organic solvents. Therefore, the spectrophotometric methods are frequently used for qualitative and quantitative determination analyte in pure form and pharmaceutical formulation [6-8].

 

Many analytical methods have been reported to estimate TH in pharmaceutical formulation and biological matrix. This method includes UPLC [9], HPLC [10-15], HPTLC [16-19], LC-MS/MS [20-24] and UV-Spectrophotometry [25-33].

 

Literature survey revealed that so far no report is available on a determination of TH using the area under curve technique with adequate sensitivity and accuracy. Therefore the scientific novelty of the present study is to established and validated fast and sensitive UV-Spectrophotometric method for estimation of TH in pure form and tablet dosage form using area under curve (AUC) technique.

 

2.     Experimental:

2.1 Chemical and reagents:

Tamsulosin hydrochloride was gifted by Spica Lab; (Ahmadabad, India) was used as the standard. The pharmaceutical preparation of TH was procured from the manufacturer (Tamsulosin hydrochloride Tablets 0.4mg spice Lab, India). Methanol was of HPLC grade and purchased from Merck Chemicals Ltd, (Mumbai, India) and distilled water was prepared from local distillation system which was filtered using 0.45μm filter (Millifilter, Milford, MA, USA).

 

2.2 Instrumentation:

The double beam UV/Vis-Spectrophotometer (UV-2450, Shimadzu, Japan) equipped with a photomultiplier detector and deuterium lamp with UV Probe 2.21 software was used for data analysis. An electronic balance (Shimadzu AUX 120) was used for weighing samples.

2.3 Selection of solvent:

The selection of solvent was done after checking the solubility of a pure drug in different solvents and finally, a mixture of methanol and water (30:70%) were selected as a solvent for establishing spectral characteristics of TH .

 

2.4 Preparation of stock solution:

A stock solution of TH was prepared by dissolving 10 mg pure drug to a clean and dry 100mL of volumetric flask and dissolved in a mixture of methanol and water (30:70 %) to obtainthe resulting solution of 100μg/mL.

 

2.5 Selection of wavelength for AUC:

For the selection of wavelength range for analysis of TH, from the above-prepared stock solution, 1mL of solution was accurately taken and transferred into 10mL of volumetric flask followed by volume adjustment upto the mark with mixture of methanol and water (30:70 %) to obtained concentration of 10μg/mL and scanned in the UV spectrum mode from 200-400 nm. From the UV spectrum of TH, AUC in the wavelength range of 220-227.60nm was chosen for the analysis. The AUC spectrum of TH is depicted in Figure 2.

 

Figure 2: AUC spectrum of Tamsulosin hydrochloride

 

2.5 Linearity study:

Linearity was studied in the range of 5- 35μg/mL. The solutions of these concentrations were prepared by diluting 0.5 -3.5mL of stock solution to 10 mL mark with the same solvent. The area of the drug was measured at 220-227.60nm. The calibration curve was constructed by plotting AUC versus concentrations for and the standard deviations of slope and intercept for the calibration plots were studied. The results of the calibration curve are presented in Table 1.

 

Table 1: Linearity study

Sr. No

Concentrations (μg/mL)

AUC

1

5

0.0105

2

10

0.0262

3

15

0.0433

4

20

0.0594

5

25

0.0758

6

30

0.0853

7

35

0.0986

n= number of determinations

 

2.6 Analysis of marketed formulation of Tamsulosin hydrochloride:

The established UV-Spectrophotometric approach was subjected for estimation of TH in pharmaceutical preparation. Marketed preparation of TH tablets was acquired from the Indian market was evaluated for the amount of TH present in the dosage form. Twenty tablets were weighed and powder in a mortar and pestle. Powder drug equivalent to 10mg of TH was transferred into 100mL of volumetric flask consisting of 30mL of a mixture of methanol and water (30:70%) and the contents of the flask were sonicated for 15 min to ensure complete solubility of the drug. Finally, the volume was adjusted up to 100ml with a mixture of methanol and water (30:70%). The resulting solution was thoroughly mixed and filtered through a 0.45μm membrane filter. From this, a 15μg/mL concentration solution was prepared after appropriate dilution. The AUC of the resulting solution was measured and the concentration of TH was calculated using a linear regression equation.

 

2.7. Validation of method:

The established UV-Spectrophotometric approach was validated according to ICH Q2 R1 guidelines [34] for different parameters like accuracy, precision, repeatability, limit of detection and of quantification and ruggedness

 

3.    RESULT AND DISCUSSION:

3.1 Accuracy:

The accuracy of the method was checked with respect to % recovery. The accuracy study of established approach was executed using standard addition method by three different solutions consisting of 12, 15 and 18μg/mL of TH. The observed % recovery and % RSD were found within the range of 99.10-100.07% and 0.65-0.82%. The results of an accuracy study meet the acceptance criterion of the study therefore the established method is reliable. The results are reported in Table 2.

 

3.2 Precision:

The precision study was examined for intra-day precision, inter-day precision and repeatability. The three different concentrations 15, 20 and 25μg/mL of TH analyzed at different time intervals in the same day for inter-day precision and repetition for three different days for a period of a week. The established method shows excellent precision which was less than 2% and % RSD for intra-day precision and inter-day precision was found to be in the range of 0.45-0.61% and 0.34-0.78%. The results are reported in Table 2

 

3.3 Repeatability:

The repeatability of the established method was checked by assessing the concentration of 15μg/mL and results was found to be less than 2%. The results are reported in

 

Table 2.

3.4. Limit of detection and quantification:

The limit of detection (LOD) and limit of quantification (LOQ) was measured using the slope of the calibration plot (S) and the standard deviation of the AUC and by a formula. The formulae used were to calculate LOD = 3.3  SD/S and LOQ = 10  SD/S. The six different concentrations in the range of 5-10μg/mL were taken and LOD and LOQ values for the established method were found to be in the range of 4.50μg and 13.64μg.

 

3.5 Ruggedness:

The ruggedness of commenced method was evaluated to measure the reproducibility of test results keeping the exactly similar operational and environmental conditions and with two different analysts. The concentration of 15 μg/mL was chosen to assess the ruggedness of the method and % RSD value was calculated. The result of ruggedness was found to be within the limit. The results are reported in Table 2.

 

Table 2: Summary of validation Parameters

Sr. No

Parameters

Results

1.

Accuracy

99.10-100.07 %

2.

 Precision

 

Intra-day precision

99.10-100.07 %

 

Inter-day precision

0.34-0.78 %.

3.

Repeatability

0.81

4.

Limit of detection

4.50 μg

Limit of quantification

13.64 μg

5.

Ruggedness

 

Analysts-I

98.48 ± 0.88

 

Analysts-II

98.27 ± 0.80

 

3.6 Analysis of marketed formulation of Tamsulosin hydrochloride:

The amount of drug was estimated (TH Tablets 0.4mg Spica Lab, India) was 98.53% and none of the excipients present in the formulation interfered with an analyte. The results are shown in Table 3. The present work was also compared to those obtained by the reported method shown in Table 4 [31].

 

Table 3: Analysis of marketed formulation

Drug

Marketed formulation

% Amount found ± SD

TH

TH Tablets 0.4 mg

98.53 ± 0.62 %

 

Table 4: Statistical Comparison with reported methods.

Comparison

Assay

% Recovery

Present work

100.25 %

98.65-99.87 %

Vijaykumar V. Rupapara M et al.

102.50 %

99.24-100.93 %

 

4.    CONCLUSION:

The developed zero-order area under curve UV spectrophotometric method for the determination of tamsulosin hydrochloride in pure form and tablet formulation using a mixture of methanol and water (30:70%) showed the excellent determination of it. However, the present study was also compared with the reported method and the result shows that the method was comparable. The established method enables the determination of drug from pharmaceutical preparation without any interference from excipients. Further, the method was validated and according to results, the commenced method is accurate, precise, rugged and sensitive.

 

5. ACKNOWLEDGEMENTS:

The authors are thankful to Cipla Ltd, India for providing drug as a gift sample. We thanks to Principal of R. C. Patel Institute of Pharmaceutical Education and Research, Shirpur, India for providing the necessary laboratory facility

 

6. CONFLICT OF INTEREST:

Authors do not have conflict of interest.

 

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Received on 31.01.2020       Modified on 27.02.2020

Accepted on 06.04.2020      ©Asian Pharma Press All Right Reserved

Asian J. Pharm. Ana. 2020; 10(2): 86-90.

DOI: 10.5958/2231-5675.2020.00015.0