Undergraduate Research

Undergraduate Research Projects

Undergraduate Research Projects  academic year 2012/13.

  1. Pre-formulation studies for omeprazole tablets

M. Ratansi, C. Migoha, , V. Manyanga, E. Kaale

 

Background information

Pre-formulation is the first step in the rational formulation of an active pharmaceutical ingredient (API). It is an investigation of the physical-chemical properties of the drug substance, alone and in combination with excipients.Omeprazole magnesium is used as an antiulcer drug and against other acid – related diseases.

 

Objective

The aim of this study is to determine the physical characteristics and identify possible interactions between Omeprazole Magnesium with its potential excipients.

 

Methods

During the study, physical characteristics of omeprazole magnesium powder were conducted which include bulk density, tapped density and sieve analysis and the possible interactions between Omeprazole magnesium and excipients were evaluated by examining the pure drug and drug-excipient powder mixtures which were stored under different conditions for a period of 90 days using Appearance, Moisture content, Near Infrared (NIR) absorption spectra and Assay by using High Performance Liquid Chromatography (HPLC).                               

 

Results

Physical characteristics: Hausner ratio = 1.2 & Compressibility Index (%) = 17.5 % hence flowability is fair. Sieve analysis-d50 value of Omeprazole magnesium is 100 µm hence it is Very fine.

Compatibility studies: Appearance and Near Infrared absorption spectra - Omeprazole magnesium alone, and Omeprazole magnesium with Sodium Lauryl Sulphate, Lactose, Avicel PH101 (microcrystalline cellulose), Starch, and Magnesium stearate remained white throughout from day 0 to day 90 in all different conditions. However in Omeprazole magnesium: Aerosil 200 (Silicon dioxide), Colour change was observed.

The Absorption NIR Spectras of Omeprazole Magnesium alone and with each potential excipient showed overlapping of spectras with the reference spectra in the entire region (350-2500nm) except for aerosil 200 whose Absorption spectra changed in the visible region of the spectrum. HPLC Assay of omeprazole magnesium alone and with all excipients showed no significant changes in omeprazole concentration for 30-day period.

 

Conclusion

The physical characteristics of Omeprazole Magnesium complied with US pharmacopeia standards with regards to the flowability and fineness, thus other excipients can be used accordingly for formulation.

The compatibility study results allow free selection of excipients except for Aerosil 200. Aerosil 200 is incompatible with omeprazole magnesium due to the reaction with magnesium.

 

 

 2. Development and Validation of an HPTLC Densitometric Method for Assay of Griseofulvin Tablets

N. Masota, P. Tibalinda, E. Kaale.

Pharm R&D Lab, The School of Pharmacy, Muhimbili University of Health and Allied Sciences, Dar Es Salaam , Tanzania

 

Background information

Griseofulvin (7-chloro-2’, 4, 6-trimethoxy-6’-methyl-Gris-2’-en-3, 4’-dione)is an oral active antifungal antibiotic derived from the mold Penicillium griseofulvum that is primarily used to treat dermatophyte infections in humans and animals.

Analysis of the Active Pharmaceutical Ingredient (API) as well as Finished Pharmaceutical Products (FPP) is of vital importance to ensure that good quality productsare manufactured and supplied to the end users.HPTLC is a simple, high throughput, relatively low cost and less time consuming technique used in qualitative and quantitative analysis of various compounds.

Literature review revealed that an HPTLC method to determine Griseofulvin in rat plasma, as well as TLC, HPLC, GLC and LC-MS methods for detection of Griseofulvin in human plasma has been developed. There is no a validated HPTLC method for quantitative and qualitative analysis of Griseofulvin tablets which has been developed.

Objective

To develop and validate an HPTLC densitometric method for determination of Griseofulvin in tablets formulation.

Methods

Ethyl Acetate, Diethyl Ether and Toluene, were obtained from Merck, Carlo Erba reagents group (German) and Scharlau chemie SA (EU).Griseofulvin sample tablets were obtained from Elys Chemical Industries Ltd (Kenya), Griseofulvin reference standards were obtained from Chifeng Pharmaceutical Co.Ltd (German).

 

HPTLC Camag Linomat V applicator (Muttenz, Switzerland), a Camag trough chamber Camag TLC scanner III, Wincats (version 1.4.3) software as data integrator and a Hamiltonn syringe (Switzerland) of 100 µL capacity. The TLC plates used for chromatographic sample separations (5×10 cm and 20×10 cm)were pre-coated with silica gel 60 F254 (Merck, Darmstadt, Germany)

Choice of mobile phase was done by observation and consideration of the polarity of different chemicals in comparison to the solubility of Griseofulvin. Stock and working solutions sample were prepared; working solutions were applied by Linomat V applicator using Hamiltonn syringe (100µL) on silica gel 60 F254 plates. The spotted plates were developed on Camag flat bottom chamber; air dried and then scanned by TLC scanner III at 299nm, validation was done as per ICH guidelines.   

  

Results

The optimal mobile phase system for Griseofulvin was Diethyl ether:Toluene (4:1) v/v, the saturation time was 25minutes.

There were no interference from the exipients or solvents, for repeatability and intermediate precision the RSD values were 1.43 and 1.58 respectively, for Linearity tests, the polynomial R2 values were 0.9915, 0.9801 and 0.9842 on three consecutive days, accuracy values tested at 80%, 100% and 120% concentrations were between 98.11% -102.66%

 Conclusion

The developed HPTLC densitometric method for Griseofulvin was simple, reproducible, accurate, cost effective and environmentallyfriendlier. The methodwas validated according to the ICH guidelines and the USP and is suitable for use in qualitative and quantitative analysis as well as screening of Griseofulvin tablets.

3. Development and Validation of HPTLC Densitometric Method for Assay of  Miconazole Cream

N. Masota,P. Tibalinda, E. Kaale.

 

Pharm R&D Lab, The School of Pharmacy, Muhimbili University of Health and Allied Sciences, Dar Es Salaam , Tanzania

 

Background information

Miconazole, ((RS)-1-(2-(2,4-Dichlorobenzyloxy)-2-(2,4-dichlorophenyl)ethyl)-1H-imidazole)is an imidazole antifungal agent, applied topically to the skin or to mucus membranes to cure fungal infections.

Analysis of the Active Pharmaceutical Ingredient (API) as well as Finished Pharmaceutical Products (FPP) is of vital importance to ensure that good quality productsare manufactured and supplied to the end users.HPTLC is a simple, high throughput, relatively low cost and less time consuming technique used in qualitative and quantitative analysis of various compounds.

The available HPTLC methods for Quantitative and qualitative analysis of Miconazole involve the use of Chloroform and Tetrachlorocarbon which are not environmental friendly.

Objective

To develop and validate an HPTLC densitometric method for determination of Miconazole in a cream formulation

Methods

Ethyl Acetate, Methanol, Ammonia solution 25% were obtained from Merck, Carlo Erba reagents group (German) and Fischer scientific UK Limited (UK). Miconazole Nitrate Cream were obtained from and Specpharm Holdings (pty) Ltd (Republic of South Africa).Miconazole reference standard were obtained from Fagron GmbH and Co. (German)

 

HPTLC Camag Linomat V applicator (Muttenz, Switzerland), a Camag trough chamber Camag TLC scanner III, Wincats (version 1.4.3) software as data integrator and a Hamiltonn syringe (Switzerland) of 100 µL capacity. The TLC plates used for chromatographic sample separations (5×10 cm and 20×10 cm)were pre-coated with silica gel 60 F254 (Merck, Darmstadt, Germany).

 

Choice of mobile phase was done by observation and consideration of the Polarity of different chemicals in comparison to the solubility of Miconazole. Stock and working solutions sample were prepared; working solutions were applied by Linomat V applicator using Hamiltonn syringe (100µL) on silica gel 60 F254 plates. The spotted plates were developed on Camag trough chamber; air dried and then scanned by TLC scanner III at 228nm,Validation was done as per ICH guidelines. 

    

Results

The optimal mobile phase system was 25ml Ethyl acetate +0.5ml Ammonia solution 25%, the saturation time was 25minutes.

On validation, there were no interference from exipients or solvents,for  repeatability and  intermediate precision the RSD values were 1.14 and 1.98 respectively, for linearity tests, the polynomial R2 values were 0.9809, 0.9927 and 0.9813 respectively on three consecutive days, Accuracy values tested at 80%, 100% and 120% concentrations were between 98.32 %-106.86%.

 

Conclusion

The Developed HPTLC densitometric method for Miconazole cream was simple, reproducible, accurate, cost effective and environmentallyfriendlier. The methodwas validated according to the ICH guidelines and the USP and is suitable for use in qualitative and quantitative analysis as well as screening of Miconazole Cream.

4. ASSESMENT OF QUALITY OF FERROUS SULPHATE AND FOLIC ACID TABLETS AND CAPSULES

S.Efrem, V.Manyanga E. Kaale,

 

Pharm R&D Lab, The School of Pharmacy, Muhimbili University of Health and Allied Sciences, Dar Es Salaam , Tanzania

 

Background information

Iron folic acid tablets regulated as dietary supplements and not been required to meet the same rigorous product quality performance standards as medicine therefore impaired product performance such as poor disintegration in the gastrointestinal tract, could limit their absorption as the result poor response to therapy .This study will provide information on the quality of ferrous sulphate folic acid tablets and capsules.

 

Objective

The purpose of this study was to assess the quality of ferrous sulphate folic acid tablets and capsule specifically on the disintegration time,the weight uniformityand the content of ferrous sulphate and the content of folic acid in tablets and capsules.

.

Methods

Disintegration time, weight uniformityand determination of the content of ferrous sulphate by titration method and the content of folic acid by HPTLC densitometric method in tablets and capsules was done where the instruments used included HPTLC Camag Linomat V Camag trough chamber, Camag TLC scanner III, Wincats (version 1.4.3), HPTLC plates, Disintegration tester and analytical balance. Analytical grade reagents were used which includes hydrochloric acid and sulphuric acid, Ammonium Ceric AR and ferroin Solution AR

 

Results

 Results were obtained where all samples passed the uniformity test and assay for iron and folic acid and some samples failed to disintegrate in accordance to specification in British Pharmacopeia as the result some products have poor quality.                                                                                                                                      

 

Conclusion

High percent of tablets failed to disintegrate for an hour where as high percent of capsules disintegrated within 15minutes. Tablets with the lowest price, which are given to pregnant women in hospitals, fail to disintegrate in high percentage. Therefore these tablets have poor

 

 

Undergraduate Research Projects  academic year 2011/12.

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