Estimation of Desloratidine and Montelukast by UV

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13th Oct 2017 Health Reference this

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SIMULTANEOUS ESTIMATION OF DESLORATIDINE AND MONTELUKAST IN COMBINED PHARMACEUTICAL DOSAGE FORM BY UV SPECTROSCOPY

ETTA.NAVEEN KUMAR*, D.SIREESHA, VASUDHA BAKSHI.

ABSTRACT: A simple, accurate,precise and economical procedure for simultaneous estimation of Desloratidine and Montelukast in combined tablet dosage form has been developed utilizing concept of simultaneous equation method. The method is based upon determination of Desloratidine at 269nm and Montelukast at 283nm in methanol. Different analytical parameters such as linearity, precision, accuracy and ruggedness were determined according to ICH guidelines. Deslortidine and Montelukast at their respective wavelength shows linearity in the concentration range of 5-30 mcg/ml and 2-22mcg/ml.respectively.The method was validated statistically. The results of analysis formulation given as percentage of label claim were found to be 100.4% and 101.% for Desloratidine and Montelukast respectively. Therefore, the proposed method can be used for the routine analysis of both drugs simultaneously in quality control laboratories.

Keywords : Desloratidine, Montelukast,simultaneous estimation, methanol

INTRODUCTION:

Desloratidine(DES) is chemically 8- chloro-6, 11-dihydro-11-(4-piperdinylidene)- 5H benzo[5,6]cyclohepta[1,2-b]pyridine.Desloratidine is a anti- histamine clinically effective drug in the treatment of Asthama. It is soluble in methanol, ethanol, water and practically insoluble in acetonitrile. Montelukast (MON),is2-[1-({[(1R)-1-{03-[(E)-2-(7-chloroquinolin-2-yl)ethenyl]phenyl}-3-[2-(2-hydroxypropan-2-)phenyl]propyl]sulfanyl}methyl)cyclopropyl]acetic acid is a widely used as Anti-arrhythmatic and Anti-asthamatic agents. Montelukast and Desloratidine is available in combined dosage forms as film coated tablets (MONDESLOR). Each tablet contains 10mg of Montelukast and 5 mg of Desloratidine. It is used for the treatment of Asthma.

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For this combination derivative spectroscopic methods and reverse phase liquid chromatographic methods are reported. However ,there is no work reported on combination of these drugs by simultaneous equation method. Hence fast, simple, and accurate spectrophotometric method was developed by applying simultaneous equation method, for the simultaneous estimation of both the drugs in tablet dosage form by uv spectrophotometry.

monte.jpg

des.jpg

MATERIALS AND METHODS:

INSTRUMENT SPECIFICATIONS: UV Spectrophotometer, Shimadzu, model 1800

CHEMICALS AND REAGENTS: Methanol obtained from local market, manufactured

Pure Deslortadine and Montelukast were obtained as gift sample from Gujarat organics Ltd,Gujarat;The tablet dosage form MONDESLOR( claim: 10mg Montelukast and 5mg Desloratidine) was procured from local market.

PREPARATION OF STANDARD STOCK SOLUTIONS:

The 10 mg of standard Montelukast and Desloratidinewere weighed accurately and transferred into 100 ml volumetric flasks seperately. They were dissolved in methanol and diluted up to the mark by using the solvent methanol to obtain a final concentration of 100μg/ml. The resulting solutions were used as a working standard solutions.

The aliquot portion of stock solutions of Montelukast and Desloratidine were diluted approximately with methanol to obtain concentration of 10 mcg/ml of each drugs.These solutions were scanned in the range of 200-400 nm in 1cm cell against blank .From the overlain spectra the wavelength selected for the estimation are 269 nm and 283nm for montelukast and desloratidine respectively.

PREPARATION OF SAMPLE SOLUTIONS

For analysis of commercial formulations 20 tablets (MONDESLOR) each cantaining 10mg of montelukast and 5mg of desloratidine were accurately weighed and the average weight was calculated and finely powdered.A quantity equivalent to 10mg of montelukast dissolved in methanol in 100ml volumetric flask and to it 5mg of desloratidine was added(standard addition method). sonicated to dissolve it completely and volume was made to the mark with methanol .mixed well and filtered through 0.45µm filter to get the final concentration of 100µg/ml. finally 10mcg/ml working concentration of each desloratidine and montelukast was prepared.

This solution was scanned over the range of 200-400 nm ,using two sampling wavelengths 269nm and 283nm determined the concentration of these drugs in tablet formulation

Using the formula.

CDES = A2ay1-A1ay2/ax2 ay1-ax1ay2

CMON = A1ay2– A2ax1/ax2ay1-ax1ay2

A1 = absorbance of formulation at 269nm.

A2 = absorbance of formulation at 283 nm.

ax1 = absorptivity of Desloratidine at 269 nm.

ax2 = absorptivity of Desloratidine at 283 nm.

ay1 = absorptivity of Montelukast at 269 nm.

ay2 = absorptivity of Montelukast at 283 nm.

CDES = concentration of Desloratidine.

CMON = concentration of Montelukast.

VALIDATION OF THE METHOD:

1) LINEARITY: Standard stock solution of Montelukast and Desloratidine: 10 mg of montelukast and desloratidine were accurately weighed and transferred into a clean and dry 100 ml volumetric flasks, dissolved with sufficient volume of methanol seperately .The volume was then made up to 100 ml with methanol to obtain the concentration of 100 μg/ml. Working standard solution: The aliquot portion of the stock solution was diluted approximately with methanol to get a concentration of 2-22 mcg/ml of montelukast and 5-30mcg/ml of desloratidine. Serial dilutions of concentration range were prepared from the working standard solution. These dilutions were scanned at the detection wavelength of 269 nm and 283nm using methanol as blank. The regression equation, Y- intercept and correlation coefficient were calculated. The linearity was thus determined and the concentration range was selected.

2) LIMIT OF DETECTION AND LIMIT OF QUANTITATION:

The LOD and LOQ were separately determined based on calibration curve. The residual standard deviation of a regression line or the standard deviation of y- intercepts of regression lines were used to calculate the LOD and LOQ.

I. Formula for LOD (μg/ml);

LOD = 3.3 x SD / S

Where,

SD = The standard deviation of the response

S = The slope of the calibration curve (mean)

II. Formula for LOQ (μg/ml);

LOQ = 10 x SD / S

Where,

SD = The standard deviation of the response

S = The slope of the calibration curve (mean)

3) ACCURACY:

The accuracy of the method was ascertained by carrying out recovery studies using standard addition method. The recovery studies are performed to determine if there was any positive or negative interference from excipients present in the formulation. The percentage recovery results revealed that the values were near to 100%, which indicates that the proposed method is accurate as the results are within the official limits. It also reveals that the commonly used excipients and additives in the formulation were not interfering with the proposed method

(Table no:4)

4) PRECISION:

Precision was found by carrying out the analysis of the standard drugs at two different concentrations in the linearity range of drugs for three times on the same day. Each concentration was applied in duplicate and % RSD was calculated (Table no :5)

RESULTS AND DISCUSSION:

Montelukast and Desloratidine showed maximum absorbance in Methanol at 269 and 283 nm.The proposed method for simultaneous estimation of both the drugs was validated as per the ICH guidelines The linearity was observed in the concentration range of 2-22 mcg/ml for montelukast and 5-50mcg/ml for Desloratidine with regression co-efficient of 0.998 and 0.998.Amount of drugs estimated by the proposed method was in good agreement with the label claim.The accuracy of the method was assessed by recovery experiments . Recovery was close to 100% for both the drugs.

CONCLUSION:

The present study comprises a UV spectroscopic method of analysis for the simultaneous estimation of montelukast and Desloratidine in tablet dosage form.From the study of validation parameters,itwas observed that the method is specific,accurate,precise,reproducible .The proposed method could be applied to routine analysis in quality control laboratories.

Table No.1 Calibration data of deslortadine.

Concentration (µg/ml)

Absorbance at 269nm

Absorbance at 283nm

5

0.187

0.111

10

0.386

0.212

15

0.559

0.309

20

0.772

0.423

25

0.960

0.520

30

1.12

0.650

Table No.2 calibration data of montelukast.

Concentration (µg/ml)

Absorbance at 269nm

Absorbance at 283nm

2

0.075

0.088

6

0.204

0.248

10

0.347

0.418

14

0.512

0.618

18

0.675

0.817

22

0.798

0.971

Table No:3 Results of analysis of tablet formulation.

BRAND

LABEL CLAIM(mg/tablet)

%LABELCLAIM

Mondeslor

Montelukast(10mg)

100.4%

Deslortadine(5mg)

101.%

Table no:4 Results of recovery studies

Drug

Amount added (mcg/ml)

Amount recovered (mcg/ml)

% Recovery

DES

80( 8)

7.96

99.5

100(10)

9.8

98

120(12)

12.2

101.6

MONT

80(8)

8.1

101.2

100(10)

9.9

99

120(12)

11.8

98.5

Table No:5 Results of precision studies.

Drug

Concentration

(µg/ml)

wavelength

Absorbance

%* RSD

DES

10

269nm

0.382

0.385

0.387

0.65

10

283nm

0.214

0.218

0.216

0.92

15

269nm

0.560

0.565

0.569

0.79

15

283nm

0.303

0.308

0.304

0.86

Drug

Concentration

(µg/ml)

wavelength

Absorbance

%* RSD

MON

10

283nm

0.413

0.415

0.418

0.60

10

269nm

0.348

0.346

0.349

0.43

14

269nm

0.510

0.509

0.512

0.29

14

283nm

0.613

0.616

0.618

0.40

* mean of three observations

Fig-1 Selection of wavelength

Fig-2 Calibration curve of montelukast:

Fig 3:calibration curve of deslortadine

REFERENCES:

SIMULTANEOUS ESTIMATION OF DESLORATIDINE AND MONTELUKAST IN COMBINED PHARMACEUTICAL DOSAGE FORM BY UV SPECTROSCOPY

ETTA.NAVEEN KUMAR*, D.SIREESHA, VASUDHA BAKSHI.

ABSTRACT: A simple, accurate,precise and economical procedure for simultaneous estimation of Desloratidine and Montelukast in combined tablet dosage form has been developed utilizing concept of simultaneous equation method. The method is based upon determination of Desloratidine at 269nm and Montelukast at 283nm in methanol. Different analytical parameters such as linearity, precision, accuracy and ruggedness were determined according to ICH guidelines. Deslortidine and Montelukast at their respective wavelength shows linearity in the concentration range of 5-30 mcg/ml and 2-22mcg/ml.respectively.The method was validated statistically. The results of analysis formulation given as percentage of label claim were found to be 100.4% and 101.% for Desloratidine and Montelukast respectively. Therefore, the proposed method can be used for the routine analysis of both drugs simultaneously in quality control laboratories.

Keywords : Desloratidine, Montelukast,simultaneous estimation, methanol

INTRODUCTION:

Desloratidine(DES) is chemically 8- chloro-6, 11-dihydro-11-(4-piperdinylidene)- 5H benzo[5,6]cyclohepta[1,2-b]pyridine.Desloratidine is a anti- histamine clinically effective drug in the treatment of Asthama. It is soluble in methanol, ethanol, water and practically insoluble in acetonitrile. Montelukast (MON),is2-[1-({[(1R)-1-{03-[(E)-2-(7-chloroquinolin-2-yl)ethenyl]phenyl}-3-[2-(2-hydroxypropan-2-)phenyl]propyl]sulfanyl}methyl)cyclopropyl]acetic acid is a widely used as Anti-arrhythmatic and Anti-asthamatic agents. Montelukast and Desloratidine is available in combined dosage forms as film coated tablets (MONDESLOR). Each tablet contains 10mg of Montelukast and 5 mg of Desloratidine. It is used for the treatment of Asthma.

For this combination derivative spectroscopic methods and reverse phase liquid chromatographic methods are reported. However ,there is no work reported on combination of these drugs by simultaneous equation method. Hence fast, simple, and accurate spectrophotometric method was developed by applying simultaneous equation method, for the simultaneous estimation of both the drugs in tablet dosage form by uv spectrophotometry.

monte.jpg

des.jpg

MATERIALS AND METHODS:

INSTRUMENT SPECIFICATIONS: UV Spectrophotometer, Shimadzu, model 1800

CHEMICALS AND REAGENTS: Methanol obtained from local market, manufactured

Pure Deslortadine and Montelukast were obtained as gift sample from Gujarat organics Ltd,Gujarat;The tablet dosage form MONDESLOR( claim: 10mg Montelukast and 5mg Desloratidine) was procured from local market.

PREPARATION OF STANDARD STOCK SOLUTIONS:

The 10 mg of standard Montelukast and Desloratidinewere weighed accurately and transferred into 100 ml volumetric flasks seperately. They were dissolved in methanol and diluted up to the mark by using the solvent methanol to obtain a final concentration of 100μg/ml. The resulting solutions were used as a working standard solutions.

The aliquot portion of stock solutions of Montelukast and Desloratidine were diluted approximately with methanol to obtain concentration of 10 mcg/ml of each drugs.These solutions were scanned in the range of 200-400 nm in 1cm cell against blank .From the overlain spectra the wavelength selected for the estimation are 269 nm and 283nm for montelukast and desloratidine respectively.

PREPARATION OF SAMPLE SOLUTIONS

For analysis of commercial formulations 20 tablets (MONDESLOR) each cantaining 10mg of montelukast and 5mg of desloratidine were accurately weighed and the average weight was calculated and finely powdered.A quantity equivalent to 10mg of montelukast dissolved in methanol in 100ml volumetric flask and to it 5mg of desloratidine was added(standard addition method). sonicated to dissolve it completely and volume was made to the mark with methanol .mixed well and filtered through 0.45µm filter to get the final concentration of 100µg/ml. finally 10mcg/ml working concentration of each desloratidine and montelukast was prepared.

This solution was scanned over the range of 200-400 nm ,using two sampling wavelengths 269nm and 283nm determined the concentration of these drugs in tablet formulation

Using the formula.

CDES = A2ay1-A1ay2/ax2 ay1-ax1ay2

CMON = A1ay2– A2ax1/ax2ay1-ax1ay2

A1 = absorbance of formulation at 269nm.

A2 = absorbance of formulation at 283 nm.

ax1 = absorptivity of Desloratidine at 269 nm.

ax2 = absorptivity of Desloratidine at 283 nm.

ay1 = absorptivity of Montelukast at 269 nm.

ay2 = absorptivity of Montelukast at 283 nm.

CDES = concentration of Desloratidine.

CMON = concentration of Montelukast.

VALIDATION OF THE METHOD:

1) LINEARITY: Standard stock solution of Montelukast and Desloratidine: 10 mg of montelukast and desloratidine were accurately weighed and transferred into a clean and dry 100 ml volumetric flasks, dissolved with sufficient volume of methanol seperately .The volume was then made up to 100 ml with methanol to obtain the concentration of 100 μg/ml. Working standard solution: The aliquot portion of the stock solution was diluted approximately with methanol to get a concentration of 2-22 mcg/ml of montelukast and 5-30mcg/ml of desloratidine. Serial dilutions of concentration range were prepared from the working standard solution. These dilutions were scanned at the detection wavelength of 269 nm and 283nm using methanol as blank. The regression equation, Y- intercept and correlation coefficient were calculated. The linearity was thus determined and the concentration range was selected.

2) LIMIT OF DETECTION AND LIMIT OF QUANTITATION:

The LOD and LOQ were separately determined based on calibration curve. The residual standard deviation of a regression line or the standard deviation of y- intercepts of regression lines were used to calculate the LOD and LOQ.

I. Formula for LOD (μg/ml);

LOD = 3.3 x SD / S

Where,

SD = The standard deviation of the response

S = The slope of the calibration curve (mean)

II. Formula for LOQ (μg/ml);

LOQ = 10 x SD / S

Where,

SD = The standard deviation of the response

S = The slope of the calibration curve (mean)

3) ACCURACY:

The accuracy of the method was ascertained by carrying out recovery studies using standard addition method. The recovery studies are performed to determine if there was any positive or negative interference from excipients present in the formulation. The percentage recovery results revealed that the values were near to 100%, which indicates that the proposed method is accurate as the results are within the official limits. It also reveals that the commonly used excipients and additives in the formulation were not interfering with the proposed method

(Table no:4)

4) PRECISION:

Precision was found by carrying out the analysis of the standard drugs at two different concentrations in the linearity range of drugs for three times on the same day. Each concentration was applied in duplicate and % RSD was calculated (Table no :5)

RESULTS AND DISCUSSION:

Montelukast and Desloratidine showed maximum absorbance in Methanol at 269 and 283 nm.The proposed method for simultaneous estimation of both the drugs was validated as per the ICH guidelines The linearity was observed in the concentration range of 2-22 mcg/ml for montelukast and 5-50mcg/ml for Desloratidine with regression co-efficient of 0.998 and 0.998.Amount of drugs estimated by the proposed method was in good agreement with the label claim.The accuracy of the method was assessed by recovery experiments . Recovery was close to 100% for both the drugs.

CONCLUSION:

The present study comprises a UV spectroscopic method of analysis for the simultaneous estimation of montelukast and Desloratidine in tablet dosage form.From the study of validation parameters,itwas observed that the method is specific,accurate,precise,reproducible .The proposed method could be applied to routine analysis in quality control laboratories.

Table No.1 Calibration data of deslortadine.

Concentration (µg/ml)

Absorbance at 269nm

Absorbance at 283nm

5

0.187

0.111

10

0.386

0.212

15

0.559

0.309

20

0.772

0.423

25

0.960

0.520

30

1.12

0.650

Table No.2 calibration data of montelukast.

Concentration (µg/ml)

Absorbance at 269nm

Absorbance at 283nm

2

0.075

0.088

6

0.204

0.248

10

0.347

0.418

14

0.512

0.618

18

0.675

0.817

22

0.798

0.971

Table No:3 Results of analysis of tablet formulation.

BRAND

LABEL CLAIM(mg/tablet)

%LABELCLAIM

Mondeslor

Montelukast(10mg)

100.4%

Deslortadine(5mg)

101.%

Table no:4 Results of recovery studies

Drug

Amount added (mcg/ml)

Amount recovered (mcg/ml)

% Recovery

DES

80( 8)

7.96

99.5

100(10)

9.8

98

120(12)

12.2

101.6

MONT

80(8)

8.1

101.2

100(10)

9.9

99

120(12)

11.8

98.5

Table No:5 Results of precision studies.

Drug

Concentration

(µg/ml)

wavelength

Absorbance

%* RSD

DES

10

269nm

0.382

0.385

0.387

0.65

10

283nm

0.214

0.218

0.216

0.92

15

269nm

0.560

0.565

0.569

0.79

15

283nm

0.303

0.308

0.304

0.86

Drug

Concentration

(µg/ml)

wavelength

Absorbance

%* RSD

MON

10

283nm

0.413

0.415

0.418

0.60

10

269nm

0.348

0.346

0.349

0.43

14

269nm

0.510

0.509

0.512

0.29

14

283nm

0.613

0.616

0.618

0.40

* mean of three observations

Fig-1 Selection of wavelength

Fig-2 Calibration curve of montelukast:

Fig 3:calibration curve of deslortadine

REFERENCES:

  1. FDA Guidance for Industry. Analytical Procedures and Methods Validation (draft guidance), August 2000.
  2. ICH guidelines Q1A (R2). Stability Testing of New Drug Substances and Products (revision 2), November 2003.
  3. ICH Q2 (R1). Validation of Analytical Procedures: Text and Methodology. International Conference on Harmonization of Technical Requirements for the Registration of Pharmaceutical for Human Use, Geneva, Switzerland. (2005).
  4. International Conference on Harmonization. Photo stability testing of new drug substance and products Q1B. International Conference on Harmonization, IFPMA, Geneva, 1996.
  5. ICH Guidance on Analytical Method Validation, in: Proceedings of the International Convention on Quality for the Pharmaceutical Industry, Toronto, Canada, and September, 2002.
  6. Konam K, Hariprasad P, Lukaraju PS, Sirajudeen MA, Fareedullah MD, Ahmed I. Determination of Montelukast sodium and Levocetrizine hydrochloride by using HPTLC method. Elixir Online J. 2012 Feb; 16.
  7. Kumar BVVS, Mathur P, Rajesh N, Rao ND, Satyanarayana P. Analytical method development and validation of Levocetirizine hydrochloride and Montelukast sodium in combined tablet dosage form by RP-HPLC. Int J Adv Pharm Res. 2011 July; 2(7): 380-96.
  8. Choudhari V, Kale A, Abnawe A, Kuchekar B, Gawli A, Patil N. Simultaneous determination of Montelukast sodium and Levocetirizine dihydrochloride in pharmaceutical preparation by derivative spectroscopy. Int J Pharm Tech Res. 2010 Jan-Mar; 2(1)
  9. Radhakrishna T, Narsaraju A, Ramakrishna M, Satyanarayna A, (2002) simultaneous determination of Montelukast and Loratadine by HPLC and derivative spectrophotometric pharmaceutical formulation. J Pharm Bio Anal.2003;31:359-68
  10. Bondili S, Reddy SP. Spectroscopic method for determination of Desloratadine in bulk and its tablet dosage forms. Int J Pharm Res. 2011; 1(2): 131-4.
  11. Mallapu Rani E, Ahad HA, Sreenivasulu R, Rani M, Mandava G, Reddy B. KK, Kranthi G. Spectrophotometric determination of Desloratadine in pharmaceuticals by using difference spectrophotometric method. J Pharm Res. 2011; 4(3): 730-1.

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