DEVELOPMENT AND VALIDATION OF SITAGLIPTINE BY VISIBLE SPECTROPHOTOMETRIC IN BULK AND PHARMACEUTICAL DOSAGE FORMS

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About Author: V. Ranjith Kumar*, Chintalapti Sujitha
* Department of Pharmaceutical Analysis,
Priyadarshini college of Pharmaceutical Sciences,
Chowdaryguda, Narapalli, Ghatkesar (Mo),
RR-District-501301. AP-INDIA.

Reference ID: PHARMATUTOR-ART-1062

Abstract
A simple, accurate, cost effective and reproducible spectrophotometric method has been developed for the estimation of Sitagliptine in bulk and pharmaceutical dosage form. Visible spectrophotometric method, which is based on measurement of absorption at maximum wavelength 540 nm. The accuracy of the methods was assessed by recovery studies and was found to be ranging from 99.5-101.5 .The developed method was validated with respect to linearity, accuracy (recovery), precision and specificity. Beers law was obeyed in the concentration range of 25-125 µg/ml having line equation y = 0.026x + 0.016 with correlation coefficient of 0.999. Results of the analysis were validated statistically and by recovery study.

Introduction
Like vildagliptin, sitagliptine is an inhibitor of the enzyme dipeptidylpeptidase - 4, an enzyme responsible, among other roles, for the degradation of the incretin hormone glucagon-like peptide-1 (GLP-1 insulinotropin), which plays a role in regulating insulin secretion. It is used in the treatment of type 2 diabetes mellitus, as monotherapy or as dual therapy with metformin, a sulfonylurea, or a thiazolidinedione. Triple therapy using sitagliptin with metformin and a sulfonylurea may be given if dual therapy is inadequate. Sitagliptin is given as the phosphate, but doses are in terms of the base 128.5 mg of sitagliptine phosphate is equivalent to about 100 mg of sitagliptine. The usual oral dose is the equivalent of 100 mg of sitagliptine once daily, as monotherapy or in combination. When given with metformin in a combination preparation, sitagliptine may be given in 2 divided doses. The dose of sulfonylurea may need to be lowered when used with sitagliptine. Sitagliptine may be taken with or without food. Dosage should be adjusted in patients with renal impairment.


Chemical structure of Sitagliptine

Adverse effects reported with sitagliptin include upper respiratory-tract infections, headache, and nasopharyngitis. Hypersensitivity reactions including anaphylaxis, angioedema, urticaria, rash, and Stevens-Johnson syndrome have also been reported.

EXPERIMENTAL DETAILS
Instruments used
A Systronics Double beam UV visible spectrophotometer 2201 with 1 cm matched quartz cells was used for all spectral and absorbance measurements. A systronics digital pH meter was used for all pH measurements.

SPECTROPHOTOMETRIC METHOD DEVELOPED FOR THE ASSAY OF SITAGLIPTINE (STG) IN BULK FORMS

Preparation of standard drug solution
About 100mg Sitagliptine was dissolved in small quantity of water in a separating funnel containing 10ml of 10% sodium carbonate add 10ml of chloroform to the above solution allow separating and collecting the chloroform layer and evaporate it to dryness and then make up to 100ml with acetone.

Preparation of Reagents
All the chemicals and reagents used were of analytical grade and solutions were prepared in double distilled water. The procedures for preparation of the various reagents were mentioned below Table No.1

Table No.1- REAGENT PREPARATION

S.No

Reagent

Preparation

1

2,3dichloro5,6dicyano-p benzoquinone(DDQ)

Dissolve 400mg of DDQ in a mixture of 20 ml of 1,4 dioxane and 40 ml of acetone and make up to 100 ml with acetone.

2

Na2CO3

 

About 1 g of sodium carbonate was accurately weighed and dissolved in 10 ml of distilled water.

Recommended procedures:
Based on the results obtained in different trials described under results and discussion in this chapter the following procedures were recommended for the determination of STG in bulk and pharmaceutical dosage formulations.

For bulk samples
Aliquots of working standard solution of Sitagliptine ranging from 0.25-1.25ml were transferred in to a series of 10ml volumetric flasks. To these 1ml of DDQ reagent was added. The total volume was adjusted to 10ml with acetone. The absorbance of the yellow colored chromogen was measured at 440 nm against reagent blank and the amount of Sitagliptine present in the sample was computed from its calibration curve. The optical characteristics are summarized in Table no.2

Table No.2: ABSORPTION MAXIMA

Reagent/Solvent

:

2,3dichloro5,6dicyano-p benzoquinone(DDQ)

Chemical principle involved

:

Molecular Salt Formation

λ max

:

440nm

Beer’s Law Limits

:

25-125µg/ml

RESULTS AND DISCUSSION
Spectral Characteristics
In order to ascertain the optimum wavelength of maximum absorption (λmax), the spectra were scanned in the wavelength region of 360-800 nm against a corresponding reagent blank.
The reagent blank absorption spectrum of each method was recorded against solvent employed in each proposed method. The absorption spectra’s, calibration curves and Ring-bom12 plots of the proposed methods are graphically represented in figures 1 to 3.

Optical characteristics
For each method the optical characteristics such as absorption maximum, Beer’s law limits, molar absorptive, sandell’s sensitivity and photometric range were presented in Table no.3. The absorption spectras of the systems are illustrated as figures 1 to 3.


 

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