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Method Development and Validation of Gliclazide in API and its Pharmaceutical Dosage Form by Uv-Visible Spectrophotometry

Jugasmita Khatua, K Vanitha Prakash, G Manasa and R Praveena

Department of Pharmaceutical Chemistry, SSJ College of Pharmacy, Vattinagulapally, Gandipet, Andhra Pradesh, India

*Corresponding Author:
Department of Pharmaceutical Chemistry
SSJ College of Pharmacy, Vattinagulapally
Gandipet, Andhra Pradesh, India

Received: 18/04/2014 Accepted: 13/05/2014 Published: 07/05/2014

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Abstract

A simple, accurate, sensitive and reproducible visible spectrophotometric method has been developed for the determination of Gliclazide in bulk and also in its pharmaceutical dosage form. The proposed method was based on ion-complex of the drug with Bromo Cresol Green showing absorbance maxima at 411 nm respectively. Beer's law was obeyed in the range of 50-300 μg/mL , with molar absorptivity 1.044x 103 L.mol-1cm-1, relative standard deviation of the method was less than 1% and accuracy (average recovery %) was 94. All the variables were studied to optimize the reaction conditions. No interference was observed in the presence of common pharmaceutical excipients. The validity of the methods was tested by analyzing the drug in its pharmaceutical preparations. Good recoveries were also obtained. The developed method employed was successful for the determination of Gliclazide in various pharmaceutical preparation.

Keywords

Gliclazide, UV-Visible Spectrophotometric Method, Bromo Cresol Green(BCG), Di Chloro Methane (DCM).

Introduction

Gliclazide [1] is an oral antihyperglycemic agent used for the treatment of non-insulin-dependent diabetes mellitus (NIDDM). Gliclazide chemically,1(Hexahydrocyclopenta(c)pyrrol-2(1H)yl)-3(p.tolylsulfonyl)urea (figure-1).

pharmaceutical-sciences-Gliclazide-chemical-structure

Figure 1: Gliclazide chemical structure.

Gliclazide is a white coloured powder, soluble in DCM, practically insoluble in water, freely soluble in methylene chloride, sparingly soluble in acetone, slightly soluble in alcohol. It belongs to the sulfonylurea class of insulin secretagogues, which act by stimulating β cells of the pancreas to release insulin. Gliclazide also has anti-platelet adhesive activity and reduces levels of free radicals, thereby preventing vascular complications.

The literature survey reveals that various methods has been reported for estimation of Gliclazide by UV spectrophotometric [2,3], RP-HPLC [4], simultaneous spectrophotometric method [5,6], HPLC [7], spectrometric method in combination with metformin [8,9], Analytical method [10].

Materials and Methods

Instrument

Elico Double Beam - Ultra Violet - Visible Double Beam Spectrophotometer SL-244 with 1cm matched quartz cells was used for all spectral measurements.

Reagents

All the chemicals used were of Analytical Reagent grade and procured from SD Fine Chemicals (SDFC), Mumbai, India.

Preparation of Acetate buffer pH 3.0

Dissolve 12 g of sodium acetate in water, add 6 ml of glacial acetic acid and dilute with sufficient water to produce 100 ml.

Preparation of 0.1% Bromo Cresol Green (BCG) dye solution for 100 ml

Weigh 0.1 gm of dye sample and dissolve in small quantity of 20% ethanol or dissolve 0.04 g in 0.58 ml of 0.1M sodium hydroxide and make up to 100 ml with water and filter it using filter paper if necessary.

Preparation of standard solution of 1mg/ml stock solution

Weigh 0.1 gm of bulk drug (Gliclazide) and dissolve in 10 ml of DCM, shake well till it dissolves and make up to 100 ml with the same.

Determination of maximum absorbance

The standard solution of Gliclazide was scanned in the range of 400-800 nm which shows maximum absorbance at 411 nm (Fig 2). Therefore, 411 nm wavelength was selected for the construction of calibration curve.

pharmaceutical-sciences-Absorption-spectrum-Gliclazide

Figure 2: Absorption spectrum of Gliclazide with Bromocresol green

Procedure for pharmaceutical preparation (Tablet)

The method was extended for the determination of Gliclazide from tablet formulation. Ten tablets of Gliclazide were accurately weighed and powdered. Tablet powder equivalent to 100 mg of Gliclazide was dissolved in 10 ml of di-chloro methane, sonicated for 15 mins and filtered. The filtrate is combined and the final volume was made to 100 ml with di-chloro methane for the above method. The solution was suitably diluted and analyzed as given under the assay procedure for bulk sample.

Results and Discussion

The chromogenic reagent is added to the drug i.e test solution and blank solution (here DCM is taken as blank) & it is shaken. To it suitable amount of chloroform and acetate buffer is added & shaken vigorously, so that the drug is extracted in chloroform layer then this is tested for absorbance in UV spectrophotometer.

The appropriate wavelength in the visible region (411 nm) was selected for the measurement of the active ingredients in the proposed method. The method was validated by linear fit curve and all the parameters were alculated. Linearity of the Gliclazide is plotted against absorbance and concentration and the linearity was graphically represented in (table 1, figure 3)

pharmaceutical-sciences-Calibration-curve

Table 1: Calibration curve

pharmaceutical-sciences-Calibration-curve-Gliclazide

Figure 3: Calibration curve for Gliclazide

The proposed method was satisfactorily applied to the determination of Gliclazide in its pharmaceutical preparations tablets, the results of the assay of the pharmaceutical preparation reveals that there is close agreement between the results obtained by the proposed method and the label claim (Table 2) and the results of the recovery values were close to 100%.

pharmaceutical-sciences-Assay-Gliclazide-Tablet

Table 2: Assay of Gliclazide in Tablet Formulation

The optical characteristics such as Maximum absorbance, Beer’s law limits, Molar absorptivity and Sandell’s sensitivity are presented in (Table 3).

pharmaceutical-sciences-Optical-Characteristics-Regression

Table 3: Optical Characteristics and Regression Analysis of the Proposed Method Developed

The regression analysis using the method of least squares was made for slope (m), intercept (b) and correlation coefficient and the results are summarized in (Table 3).

LOD and LOQ

The LOD and LOQ were calculated from the equations,

LOD =3.3 σ/S and LOQ = 10 σ/S, where σ is the standard deviation of the lowest standard concentration and S is the slope of the standard curve. The results are shown in table 3

Conclusion

The proposed method was simple, economical, sensitive, precise reliable and reproducible for the routine estimation of Gliclazide in bulk as well as in tablet formulation.

Acknowledgement

The authors are very thankful to Principal and management of SSJ College of Pharmacy for providing necessary facilities to carry out research work.

References