INTRODUCTION:

Desloratadine is a tricyclic anti histamine, which has a selective and peripheral H₁-antagonist action. It is used to treat the allergies. Structure of Desloratadine is shown in figure 1.¹

Figure 1: Structure of Desloratadine

Received on 29.04.2015 Modified on 07.05.2015

Research J. Pharm. and Tech. 8(6): June, 2015; Page 693-696

DOI: 10.5958/0974-360X.2015.00109.2

Literature review seems that there are several methods reported for estimation of desloratadine in different mobile phase that contain buffer as composition. So, alternative, simple and relatively cheap method is required for Desloratadine.^2-8

MATERIALS AND METHODS:

Instrument:

_{The HPLC used was Shimadzu LC-2010 model.}

Apparatus:

The apparatus used were volumetric flasks, pipettes, beakers, measuring cylinder. All were made of durasil and borosil.

Reagents and Chemicals:

Methanol (HPLC grade) and HPLC water were used. Desloratadine API was procured from Saga Laboratories, Ahmedabad.

Marketed formulation:

Marketed dosage form (SAGADES) was procured from Saga Laboratories, Ahmedabad.

Preparation of stock solution:

Accurately weighted quantity of 10 mg Desloratadine was transferred into 100ml volumetric flask and dissolved up to the mark with Methanol. It gives a stock solution having strength of 100µg/ml.

Preparation of sample solution:

From stock solution, accurately measured volume of Desloratadine 0.8ml, 1.2ml, 1.6ml, 2.0ml and 2.4ml were transferred to 10ml volumetric flask and volume was made up to the mark with methanol to prepare solution having concentration of 8µg/ml, 12 µg/ml, 16 µg/ml, 20 µg/ml and 24 µg/ml.

Preparation of mobile phase:

70 ml of Methanol and 30 ml of HPLC grade water were taken. It was mixed properly. Then mobile phase was filtered through 0.45µm filter paper with vacuum filtration assembly. Mobile Phase was transferred to reservoir bottle and Sonicated for 20 min.

Validation of method:

System suitability parameters like theoretical plates, tailing factor and retention time were studied by injecting five replicates of standard concentration 16 µg/ml and %RSD for retention time was calculated.

The linearity range for Desloratadine was found to be in the range of 8-24 µg/ml. Calibration curves were constructed by plotting absorbance versus concentrations of Desloratadine and calculating the regression equations.

For repeatability six replicates of one concentration 16 µg/ml of standard solution of Desloratadine was analyzed. For intraday precision three replicates of three concentrations 12 µg/ml, 16µg/ml and 20 µg/ml of standard solution of Desloratadine was analyzed at three different time intervals. For interday precision three replicates of three concentrations of 12µg/ml, 16µg/ml and 20 µg/ml standard solution of Desloratadine was analyzed at three consecutive days. The peak area was calculated at 242nm. The %RSD was calculated.

Accuracy of the method was determined by known amounts of standard solutions of Desloratadine 6.4µg/ml, 8.0µg/ml, 9.60µg/ml was added into prequantified sample solutions of 8 µg/ml. Accuracy was determined by % recovery study.

The robustness of analytical method is a measure of its capacity to remain unaffected by small but deliberate variations in the method parameters and provides an indication of its reliability during normal usage. To confirm robustness, change was done in flow rate (±0.2ml/min) and wavelength (±2 nm). The %RSD was calculated

Analysis of marketed formulation:

Twenty tablets were weighted accurately and powdered. A quantity equivalent to 5mg of Desloratadine was weighted and transferred to 100ml volumetric flask. The volume was made up to the mark with the methanol. From the above solution 1.6 ml was transferred to 10 ml volumetric flask and volume was made up to the mark with methanol. From this solution further dilutions were made to obtain concentration range 8- 24 µg/ml. 20 µl of sample solution was injected under the chromatographic conditions and the chromatogram was recorded. The amount of Desloratadine present in tablet formulation was determined by comparing the peak area from the standard.

RESULT:

Selection of wavelength:

Standard solution of Desloratadine was scanned over the range of 200 to 400nm. Maximum absorbance of drug was observed at 242nm. Hence the wavelength selected for the estimation was 242nm (figure 2).

242nm

Figure 2: UV-Spectrum of Desloratadine

Validation of HPLC method:

System Suitability:

System suitability data are shown in table 1.

Table 1: System suitability data for Desloratadine

Parameters	Result	Acceptance limit
%RSD of Retention time	0.413	<2.0
Theoretical Plate	1756.4 ± 5.78	>1500
Tailing Factor	1.33 ± 0.01	<1.5

Linearity and Range:

The HPLC method was linear over the concentration range of 8-24 µg/ml. Linearity and range data are shown in table 2. Overlay chromatogram and calibration curve are shown in figure 3 and 4 respectively.

Table 2: Linearity and range data for Desloratadine

Parameters	Result
Linearity- range	8-24 µg/ml
Regression Equation	y = 73142x + 10697
Correlation coefficient	0.9975

Figure 3: Overlay spectra of Desloratadine

Figure 4: Calibration curve of Desloratadine

Precision:

The results of repeatability, intraday precision and interday precision are shown in table 3.

Table 3: Precision data for Desloratadine

Precision	%RSD
Repeatability	0.56 %
Intraday precision	0.50-1.03%
Interday precision	0.15-0.64%

Accuracy:

Accuracy was determined by evaluating the recovery of analyte. The accuracy data are shown in table 4.

Table 4: Data of accuracy for Desloratadine

% of nominal amount	Actual amt. (µg/ml)	Spiked amt. (µg/ml)	Total amt. (µg/ml)	Amt. obtained	% recovery
80	8	6.4	14.4	14.2	98.61
100	8	8	16	15.9	99.37
120	8	9.6	17.6	17.3	98.29

Robustness:

The result obtain for different flow rate and wavelength are shown in table 5.

Table 5: Robustness data for Desloratadine

Parameters		%RSD
Different Flow rate	0.8	1.13
	1.0	0.92
	1.2	0.33
Different Wavelength	240	0.77
	242	0.73
	244	1.02

Analysis of drug in tablet dosage form:

The amount of Desloratadine present in tablet formulation was determined and %assay was calculated. Chromatogram is shown in following figure.

Figure 5: Chromatogram of Drug in Tablet dosage form

Table 6: Data for analysis of drug in Table dosage form

Dose

Amount Found (mg/tablet )

(Mean ± SD) (n = 3)

% Label Claim

(Mean ± SD) (n = 3)

5 mg

5.016 ± 0.059

100.33 ± 1.18

DISCUSSION:

A specific, accurate and precise RP-HPLC method has been developed and validated for estimation of Desloratadine in Tablet dosage form. The accuracy, precision and other validation parameters were determined and validated statistically. Parameters which were validated are as follows:

The linearity and range was found to be 8-24 μg/ml. The co-relation coefficient was found to be 0.9975. The % RSD of repeatability, intraday and intermediate precision was found to be less than 2%. The % RSD for Robustness parameters (flow rate change, wavelength change) was found to be less than 2%. So the developed method was precise and robust. The % Recovery of Desloratadine was found in the range of 98.29 % -98.6 %. The assay value for Desloratadine was found to be 99.40 % - 100.33 %. So, the developed method was accurate. The developed method can be used for estimation of Desloratadine in tablet dosage form.

List of symbol and Abbreviation:

Table 7: List of symbol and Abbreviation

Sr. No.	Serial Number
ml	Milliliter (S)
Mg	Microgram
Mm	Micrometer
Mg	Milligram
Mm	Millimeter
Nm	Nano meter
%	Percentage
v/v	Volume / volume
Min	Minute
RP-HPLC	Reverse Phase High performance Liquid Chromatography
SOP	Standard Operating Procedure
API	Active Pharmaceutical Ingredient
Amt.	Amount

ACKNOWLEDGEMENT:

We are thankful to SAGA Laboratories, Ahmedabad for providing API and formulation of Desloratadine.

REFERENCES:

1 Desloratadine: Medlineplus Drug Information URL:http://www.nlm.nih.gov/medlineplus/druginfo/meds/a602002.html.

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