chandra ppt

Views:
 
Category: Education
     
 

Presentation Description

No description available.

Comments

Presentation Transcript

PowerPoint Presentation:

1 Modified RP-HPLC Method for Simultaneous Estimation of Naproxen Sodium and Domperidone Maleate in Bulk and Pharmaceutical Dosage Form Submitted by (Reg. No : 26105521) Under the Guidance of Mr. R. Senthil kumar, M. Pharm., (Ph.D)., Department of Pharm. Analysis, Swamy Vivekanandha College of Pharmacy.

Contents:

Contents 2 Introduction Objective of the work Drug profile Materials Results and discussion Conclusion Reference Publications

PowerPoint Presentation:

3 Principle : Adsorption Types: NP- HPLC and RP-HPLC In NP- HPLC stationary phase is polar, mobile phase is nonpolar. In RP-HPLC stationary phase is non polar, mobile phase is polar. RP-HPLC is mostly used, because 90% of the drugs are polar in nature. In the pharmaceutical analysis HPLC (High performance liquid chromatography) plays major role. INTRODUCTION

PowerPoint Presentation:

4 For the present study, the drug Naproxen sodium and Domperidone maleate was selected for their estimation. The HPLC method was considered the choice of estimation, since this method is the most powerful of all chromatographic and other separative methods. Different methods have been reported for analysis of DOM by Spectrophotometry, Spectroflourimetry, and HPLC and HPTLC and for NAP, the methods reported are Spectrophotometry, Spectroflourimetry HPLC and HPTLC, either alone or in combination with other drugs. There are fewer HPLC and HPTLC methods are reported for the simultaneous analysis of NAP and DOM in their combined dosage form.

PowerPoint Presentation:

5 OBJECTIVE OF THIS WORK Development of RP-HPLC method, which allow the simultaneous, fast, routine determination of naproxen sodium and domperidone maleate in bulk drugs than the other existed methods. To validate the developed RP-HPLC method by using various analytical parameters such as accuracy, precision, specificity, robustness, ruggedness, linearity and range, limit of detection (LOD), limit of quantitation (LOQ) as per ICH guidelines(Q2R1). Application of the developed method on the most significant, commercially available Pharmaceutical dosage form.

PowerPoint Presentation:

6 DOMPERIDONE MALEATE Structure: Standard: NLT 99.0 % and NMT 101.0 % of Domperidone maleate Description: white or almost white powder, soluble in methanol, acetonitrile and slightly soluble in water. Mechanism of action: dopamine receptor blocking activity Categories: Antiemetics, Dopamine Antagonists. pKa -7.19. DRUG PROFILE

PowerPoint Presentation:

7 NAPROXEN SODIUM Structure: Standard: not less than 99.0 % and not more than 101.0 % of naproxen sodium, Description: It is a white or almost white crystalline powder, soluble in cold water and methanol. Mechanism of action: COX 1 and COX 2 Inhibitor Categories: NSAID and Gout Suppressants pKa: 4.15

PowerPoint Presentation:

8 INSTRUMENTS USED S.No Name Manufacturer/Supplier 1 Analytical Balance Satorius 2 pH Meter Shimadzu 3 HPLC Waters 4 UV Visible detector Waters CHEMICALS USED S.No Name Manufacturer/Supplier 1 Water Merck 3 Di potassium hydrogen phosphate Merck 4 Acetonitrile Merck 5 Methanol Merck 6 Di hydrogen potassium phosphate Merck MATERIALS s.no standard % purity Obtained from 1. Naproxen sodium 99.85 Kaushikh pharma therapeutic pvt ., ltd. 2. Domperidone maleate 99.80

PowerPoint Presentation:

9 Method development: λ max of Naproxen sodium : 231 nm λ max of Domperidone maleate : 286 nm Isobestic Point : 274 nm Selection of wavelength

PowerPoint Presentation:

10 Trial 1 Parameters Description Column C 18 :250X4.6 mm, 5µ Mobile Phase Water : methanol(20:80) Diluent Methanol Flow rate 1.0 ml/min Wavelength 274 nm Injection mode Auto injector (vial) Run time 30 min Chromatogram of Naproxen sodium Chromatogram of Naproxen sodium and Domperidone maleate Domperidone maleate was eluted properly but Naproxen sodium was not eluted. So the mobile phase has been changed for next trial .

PowerPoint Presentation:

11 Trial 2 Parameters Description Column C 18 :250X4.6 mm, 5µ, Mobile Phase Acetonitrile : water(70:30) Diluent Acetonitrile Flow Rate 1 ml/min Wavelength 274 nm Injection mode Auto injector (vial) Run time 20 min Chromatogram of Domperidone maleate Chromatogram of Naproxen sodium and Domperidone maleate Theoretical plates of Naproxen sodium are less. So the mobile phase has been changed for next trail.

PowerPoint Presentation:

12 Parameters Description Column C 18 :250X4.6 mm, 5µ, Mobile Phase Acetonitrile : potassium phosphate buffer (50:50) Diluent Acetonitrile Flow Rate 1 ml/min Wavelength 274 nm Injection mode Auto injector (vial) Run time 20 min Trail 3 Chromatogram of Domperidone maleate Chromatogram of Naproxen sodium and Domperidone maleate Both peaks are not eluted properly. So the mobile phase has been changed for next trail

PowerPoint Presentation:

13 Parameters Description Column C 18 :250X4.6 mm, 5µ, Mobile Phase Mixed Phosphate buffer : acetonitrile (50:50), pH-3 Diluent Mobile phase Flow Rate 1 ml/min Wavelength 274 nm Injection mode Auto injector(vial) Run time 20 min Trial 4 Chromatogram of Domperidone maleate Chromatogram of Naproxen sodium and Domperidone maleate Merged peaks were observed. So the pH was changed for next trial.

PowerPoint Presentation:

14 Parameters Description Column C 18 :250X4.6 mm, 5µ, Mobile Phase Mixed Phosphate buffer : acetonitrile (50:50), pH-6.5 Diluent Acetonitrile Flow Rate 1 ml/min Wavelength 274 nm Injection mode Auto injector (vial) Run time 20 min Chromatogram of Domperidone maleate Chromatogram of Naproxen sodium and Domperidone maleate Resolution, Theoretical plates and Symmetric factor were found to be with in the limit. So this method was finalized as the optimized method. Trial 5 (optimized method)

PowerPoint Presentation:

15 Method Validation: Preparation of Standard Stock Solutions: (Sol A) 50.88 µg/ml of DOM and 1000 µg/ml of NAP were prepared. Working standard Solution From sol A 10.17µg/ml of DOM and 200µg/ml of NAP were prepared . Preparation of Sample Stock Solutions(Sol B): Equivalent to standard 50.88 µg/ml of DOM and 1000 µg/ml of NAP were prepared. Working sample Solution From sol B 10.17µg/ml of DOM and 200µg/ml of NAP were prepared .

PowerPoint Presentation:

16 Accuracy : (standard addition method) 50% spiking 100% spiking 150% spiking 2ml sample sol A + 1ml standard sol B 2ml sample sol A + 2ml standard sol B 2ml sample sol A + 3ml standard sol B

PowerPoint Presentation:

Acceptance criteria for the percentage of the recovery should be within ± 2.5 %. In our study, the percentage recovery of naproxen sodium was found to be 98.43%, 100.52% and 98.08% from 50%, 100% and 150% sample solutions respectively. For domperidone maleate it was found to be 100.02%, 98.12% and 99.93% from 50%, 100% and 150% sample solutions respectively. 17 Drug Sample Soln (µg/ml) Spiked sample (µg/ml) Total amount (µg/ml) Amount recovered % Recovery % NAP 200 100 300 49.21 98.43 200 200 400 100.52 100.52 200 300 500 147.12 98.08 DOM 10.17 5.085 15.185 50.01 100.02 10.17 10.17 20.34 98.12 98.12 10.17 15.835 26.005 149.9 99.93

PowerPoint Presentation:

18 Precision: Working standard solution of domperidone maleate (10.17 μg/ml) and naproxen sodium (200 μg/ml) were injected six times in single day. Acceptance criteria for the precision of the method, the %RSD should not be more than 2%. In the present study the % RSD was 0.81 for DOM 0.17 for NAP

PowerPoint Presentation:

System suitability parameters Parameters Naproxen sodium Domperidone maleate Acceptance criteria Theoretical plates 6968 4074 ˃ 2000 Resolution 8.98 - ˃2 Symmetric factor 1.09 1.10 ≤ 2 All parameters were with in the limit, 19

PowerPoint Presentation:

Linearity: From the standard solution A 0.5, 1, 1.5, 2, 2.5, and 3 ml was transferred to six 10 ml flasks and made up the volume with mobile phase. The concentrations of DOM and NAP were found to be 2.54-15.264 µg/ml and 50-300 µg/ml respectively . The correlation coefficient (r 2 ) values of both drugs were found to be 0.999. The equation of regression line for DOM was found to be y = 76684x – 3531.2. The equation of regression line for NAP was found to be y = 56016x + 87257. 20

PowerPoint Presentation:

21 25% 50% 75% 100% 125% 150%

PowerPoint Presentation:

Limit of Detection (LOD) and Limit of Quantitation (LOQ): The LOD and LOQ were found out by following fromula LOD = 3.3 SD/ Slope LOQ = 10 SD/Slope The LOD and LOQ value for domperidone maleate were 0.15  g/ml, 0.50  g/ml respectively and for naproxen sodium were 5.14  g/ml, 15.42  g/ml, respectively. 22

PowerPoint Presentation:

Ruggedness: Working standard solution of domperidone maleate (10.17 μg/ml) and naproxen sodium (200 μg/ml) were injected six times in different days . Acceptance criteria for the precision of the method, the %RSD should not be more than 2% in the present study the %RSD 1.19 for DOM and 0.39 for NAP. 23

PowerPoint Presentation:

Flow rate at 0.9 ml/min Flow rate at 1.1 ml/min Robustness The % RSD was 1.64 for DOM and 1.29 for NAP The % RSD was 1.15 for DOM and 0.90 for NAP The change in flowrate has no effect on the method. 24

PowerPoint Presentation:

Acetonitrile: Phosphate buffer pH 6.5, 45:55, v/v ) Acetonitrile: Phosphate buffer pH 6.5, 55:45, v/v) The % RSD was 0.18 for DOM and 1.08 for NAP The % RSD was 0.18 for DOM and 1.08 for NAP The change in mobile phase has no effect on the method. 25

PowerPoint Presentation:

Placebo solution of Naproxen sodium and Domperidone maleate Chromatogram of marketed formulation of Naproxen sodium and Domperidone maleate Specificity: 26

PowerPoint Presentation:

The percentage recovery of naproxen sodium and domperidone maleate was found to be 99.81% and 99.6% respectively. Analysis of Pharmaceutical Dosage Form: 27

PowerPoint Presentation:

28 Conclusion: The developed and validated RP-HPLC method outlined is very obvious, affordable, dynamic, low cost, rapid and easy to perform with small sample volume and good repeatability. It can be adopted for the routine quality control analysis of simultaneous determination of naproxen sodium and domperidone maleate because of good resolution of the chromatographic peaks.

PowerPoint Presentation:

29 Shubhangi M Pawar , Bharat S Patil and Ravindra Y Patil . Validated HPTLC Method for Simultaneous Quantitation of Domperidone maleate and Naproxen sodium in Bulk Drug and Formulation. Eurasian J Anal Chem. 2010; 5(3):284-292. Shozan Mondal Md , Ahsanul Haque Md , Mohammad Safiqul Islam and Ashraful Islam SM. Development and Validation of RP-HPLC Method for the Simultaneous Estimation of Domperidone and Naproxen in Tablet Dosage Form. J Appl Pharm Sci. 2011; 1(7): 145-148 Shubhangi M Pawara , Jitendra D Fegade , and Rajesh Y Chaudhari . Validated HPLC Method for Simultaneous Quantitation of Domperidone maleate and Naproxen sodium in Bulk drug and Formulation. Der Pharmacia Lettre . 2010; 2(5):229-236. ICH Q2(R1), Harmonised Triplicate Guideline, Validation of analytical Procedures: Text and Methodology, International Conference on Harmonization ICH, Geneva. 2005. Selected References

PowerPoint Presentation:

Publications in the present work E. Chandra Sekhar, R. Senthil Kumar, M. Ravi Sankar and P. Prasanthi. Simultaneous Estimation of Naproxen Sodium and Domperidone Maleate in Bulk and Pharmaceutical Dosage Form by Modified RP-HPLC Method. International Journal of Pharmaceutical and Chemical Sciences . 2012; 1(4):1615-1623. Poster presentations “RP-HPLC Method for Simultaneous Estimation of Naproxen sodium and Domperidone maleate in Bulk and Pharmaceutical Dosage Form”, by Chandra Sekhar E, Senthil Kumar R, Prasanthi P and Sereya K at International Congress of Pharmacy Graduates 2012, held at Chettinad Health City, Chennai on 6 th and 7 th October 2012. 30

PowerPoint Presentation:

Thank you 31

authorStream Live Help