You are hereSIMULTANEOUS DETERMINATION AND VALIDATION OF TELMISARTAN AND RAMIPRIL IN PHARMACEUTICAL DOSAGE FORM BY RP – HPLC AND HPTLC

SIMULTANEOUS DETERMINATION AND VALIDATION OF TELMISARTAN AND RAMIPRIL IN PHARMACEUTICAL DOSAGE FORM BY RP – HPLC AND HPTLC


Lable Claim
TELM - 40 mg
RAMI - 5 M

Preparation of Mobile Phase Ten volumes of ethyl acetate, three volumes of chloroform and one volume of methanol are mixed thoroughly and used as mobile phase.

Diluent
Methanol and chloroform in the ratio of 1:1 is used as diluent.

Preparation of Standard Stock Solution
An accurately weighed quantity of 40 mg of Telmisartan (working standard and 5 mg of Ramipril (working standard) were dissolved in diluent [methanol and chloroform (1:1)] taken in 20ml volumetric flask. Then the volume is made up to 20 ml with diluent, having the concentration of 2 and 0.25 mg/ml for Telmisartan and Ramipril, respectively.

Preparation of Standard Solution
1m of standard stock solution is transferred to 10 ml volumetric flask. Then it is made up to volume with the diluent, having the concentration of 0.2 and 0.025 mg/ml for Telmisartan and Ramipril, respectively.

Preparation of Sample Solution
Twenty tablets are weighed and powdered. The powder equivalent to 40 mg of Telmisartan and 5 mg of Ramipril (average weight of tablet) was transferred to 20 ml volumetric flask. The contents were dissolved in diluent and the volume is made up to the mark.1m of the above solution is transferred to 10 ml volumetric flask. Then it is made up to volume with the diluent.The contents were mixed well using ultra-sonicator and filtered through Whatman filter paper number: 42.

Estimation Method
The sample was spotted on the chromplate with help of Linomate IV spotting system. The chromatograms were recorded and the peak area for TELM and RAMI area values of sample with that of standard using the formula:

                                                        Sample area x Std. Conc.x Std. Purity x
                                                       
(1000-Std.Lod) x Avg.weight

Amount of drug present            =     -----------------------------------------------------------------
in each tablet                                                   Std. area x Sample conc.x100x100

                                            Amount present

Percentage label claim  = -------------------------   x 100   

                                               Label claim

RESULTS AND DISCUSSIONS:

The assay values are tabulated in Table 1

Chromatogram of Telmisartan & Ramipril Formulation

TABLE 1

QUANTITATIVE ESTIMATION

Tablet Sample

Lable Claim (mg)

Amount present

(mg/tablet)

%Lable Claim

%Deviation

TELM


RAMI

40


5

40.20


5.0099

100.49


100.19

+ 0.49


 +0.19

Each value is mean of three readings

The values obtained for the assay are statistically validated and tabulated in Table 2

TABLE 2

STATISTICAL DATA FOR QUANTITATIVE ESTIMATION BY RP-HPLC

Tablet sample

%Label Claim (mg)

Standard Deviation

%Relative Standard Deviation

Standard Error

TELM


RAMI

100.49


100.19

±1.30


±0.1069

       1.29


       0.106

   0.750


   0.016

Validation
For validating the developed method the parameters like linearity, range, suitability, system precision and assay (recovery studies) are studied. The validation procedures are carried out as follows.

Linearity and Range
The linearity of the analytical procedure is its ability (with in given range) to obtain the test results which are directly proportional to the concentration of analyte in the sample. Linearity was assessed by performing single measurement at several analyte concentrations. A minimum of five concentrations were recommended for linearity studies.

To evaluate the linearity range of Telmisartan and Ramipril, varying concentrations of standard stock solution is diluted with mobile phase to give minimum of five concentrations in the range of 16 to 24µg/ml for Telmisartan and 2 to 3 µg for Ramipril. A calibration curve was constructed for each sample by plotting the peak area obtained against the concentration.

The linearity data for Telmisartan and Ramipril are presented as follows

TELMISARTAN
There exists a linear relationship in the concentration range of 16 to 14µg/ml for Telmisartan. The data are tabulated

Linearity of Telmisartan

LINEARITY DATA FOR TELMISARTAN

CONCENTRATION (µg/ml)

PEAK AREA

16


18


20


22


24

    3838.48


4286.70


4700.65


5237.62


5735.72

From the data obtained correlation coefficient, y-intercept and slope were calculated to provide mathematical estimates of linearity for Telmisartan and tabulated

PARAMETERS

TELMISARTAN

Linear Dynamic range


Correlation coefficient


Slope(m)


Intercept(c)

16-24µg/ml


0.9998


237.91


1.288

ANALYTICAL PERFORMANCE PARA METERS OF TELMISARTAN

RAMIPRIL
There exists a linear relationship in the concentration range of 2 to 3µg/ml for Ramipril. The data are tabulated in Table 4a

Linearity of Ramipril

CONCENTRATION(µg/ml)

PEAK AREA

2.00

2.25

2.50

2.75

3.00

2200.66

2450.88

2725.44

2995.46

3264.802     


LINEARITY DATA FOR RAMIPRIL

from the data obtained correlation coefficient, y-intercept and slope were calculated to provide mathematical estimates of linearity for Ramipril and tabulated


PARAMETERS


RAMIPRAMIL

Linear Dynamic range


Correlation coefficient (r)


Slope (m)


Intercept (c

2 – 3 µg/ml


0.999


1088.6


4.8739

SUITABILITY
System suitability parameters are tabulated in Table 5

           Parameter

TELM

RAMI

Resolution

4.38

Asymmetry factor

 1.48

 1.56

No. of Theoretical plates

 2945

4738

Tailing factor

 1.2

1.

TABLE -5 - SYSTEM SUITABILITY

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