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COURSE TITLE: PHARMACEUTICAL ANALYSIS IV
COURSE NO: PHARM -4121
An Assignment
on
Different Dosage forms With their Quantitative
and Qualitative Evaluation
Submitted to:
Dr. Md. Golam Hossain,
Professor,
Pharmacy Discipline,
Khulna University
Submitted by:
Sk. Tanvir Raihan Emon
171111
Pharmacy Discipline
Khulna University
Dosage Form
Dosage forms are pharmaceutical drug products in the
form in which they are marketed for use , with a specific
mixture of active ingredients and inactive components, in
a particular configuration, and apportioned into a
particular dose.
For Example: Tablets, capsules , syrups etc.
Types of Dosage Forms
Depending on the
physical form
Solid Semisolid Liquid gaseous
Types of Dosage Forms
Depending on
route of
administration
1. Oral
2. Topical
3. Rectal
4. Vaginal
5. Parenteral
6. Inhaled
7. Optic
8. Opthalmic
Oral Dosage Forms
1.Tablet:
Tablet is a hard, compressed medication in round, oval or square
shape. It mainly includes excipients such as binders,
disintegrates, coating materials, sweeteners, disintegrates,
glidants.
For Example: Paracetamol Tablet, Antacid Tablet, Disprin Tablet
Some
subtypes
of tablet
1. Compressed Tablet. Produced in large scale with a great pressure. Ex-Paracetamol
2. Coated Tablet. Has a covering over a tablet. Ex- Riboflavin
3. Buccal tablet. Administered by placing them in the mouth. Ex- Nitroglycerin
4. Effervescent Tablet. Designed to dissolve in water, and release carbon dioxide. Ex- Disprin
5. Chewable Tablet. Are chewed within the buccal cavity prior to swallowing. Ex- Antacid
6. Dental cone. Ex- Dental miror
7. Pastilles.
Oral Dosage Forms
2. Capsules:
Capsule is a medicine contained in a water-soluble gelatin shell..
The shell is used to protect the API from degradation due to any
gastric materials. There are generally two types of capsules.
For Example: Doxicap (Doxicycline capsules)
Liquid Preparations
3. Gargles and mouth washes
These are liquid preparations, mainly used to prevent oral or throat
infections. Ex- Listerine mouth wash
4. Oral Suspension
Oral suspensions are liquid solution where solid active ingredients remain
suspended inside the vehicle of the container. This medication are needed
to be shaken before use other wise the medications will settle down and
the mixture will not be homogenous. Ex- Phenytoin suspensions.
Topical Preparations
5. Ointments
These are semi solid greasy preparations for application in skin ,
rectum, vagina or in nasal mucosa. Example: Clobetasol Propionate
ointment.
6. Pastes
These are mainly ointments with a high concentration of fine solid
particles. Ex- 30% salicylic acid
Parenteral Preparations
7. Intravenous
It’s a liquid administered directly into the bloodstream via a vain. The solution
must be sterile. The biggest advantage of IV preparations is that as there are no
absorption phases, the drug is rapidly distributed to give quick action inside the
body. Ex- Glucose preparations
8. Intramuscular
It is the injection of a liquid directly into the muscle. Ex- Different vaccines are
made as IM preparations, Like BCG vaccine.
9. Subcutaneous injection
In this injection, the liquid is directly pushed into the cutis, the layer below
dermis and epidermis of skin. Ex- Insulins
10. Ophthalmic preparations
These medications are generally liquid or semi solid cream in nature and are
intended for application to the conjunctiva or the eyelids. They are used to prevent
eye infections and so must be sterile. Ex- Vaseline.
11. Rectal Preparations
Rectal medicines are medications prepared specifically for insertion into
the rectum. They are compounded in many forms. Among them the most popular
and widely used are suppositories which are prepared by mixing medicine with a
wax-like substance to form a semi-solid, bullet-shaped form that will melt after
insertion into the rectum. Ex: Paracetamol suppositories
Qualitative assay of
different pharmaceutical dosage form
Aciclovir Oral Suspension Assay
Procedure:
1. To a weighed quantity containing 0.4 g of Aciclovir add 400 ml of water and 25 ml of 1M
sulphuric acid , shake well, disperse with the aid of ultrasound for 10 minutes and add
sufficient water to produce 500 ml.
2. Filter the resulting solution, discard the first few ml of filtrate and dilute 5 ml of the
filtrate to 200 ml with 0.05M sulphuric acid .
3. Add 10 ml of the resulting solution to 5 ml of a 0.01% w/v solution of cetrimide in 0.05M
sulphuric acid add sufficient 0.05M sulphuric acid to produce 100 ml and measure the
fluorescence, Appendix II E, using an excitation wavelength of 308 nm and an emission
wavelength of 415 nm.
4. Set the instrument to zero using a 0.0005% w/v solution of cetrimide in 0.05M sulphuric acid .
5. Calculate the content of C8H11N5O3 in the oral suspension from the fluorescence obtained by
carrying out the operation at the same time using a mixture prepared by adding 10 ml of a 0.002%
w/v solution of aciclovir BPCRS in 0.05M sulphuric acid and beginning at the words to 5 ml of a
0.01% w/v solution of cetrimide ...'. Determine the weight per ml of the oral suspension, Appendix
V G and calculate the content of C8H11N5O3, weight in volume, using the declared content of
C8H11N5O3 in aciclovir BPCRS .
Source: Volume 3, page no:7919 (Brithish pharmacopeia 2009
Benzoyl Peroxide Cream Assay
Procedure:
1. Mix a quantity of the preparation being examined containing the equivalent of
0.25 g of anhydrous benzoyl peroxide with 50 ml of acetone and add sufficient
acetone to produce 100 ml.
2. To 10 ml add 25 ml of a 20% w/v solution of potassium iodide , mix, stopper the
flask and allow to stand for 15 minutes protected from light.
3. Add 25 ml of acetone and titrate with 0.01M sodium thiosulphate VS using starch
mucilage , added towards the end of the titration, as indicator.
4. Repeat the operation without the substance being examined. The difference
between the titrations represents the amount of sodium thiosulphate required.
5. Each ml of 0.01M sodium thiosulphate VS is equivalent to 1.211 mg of C14H10O4.
Source: Volume 3, page no:8088 (British pharmacopeia 2009)
Quantitative assay of
different pharmaceutical dosage form
Potentiometric Titration
 Potentiometric titration is a laboratory method to determine the concentration
of a given analyte. It is used in the characterization of acids. In this method,
there is no use of a chemical indicator. Instead, the electric potential across the
substance is measured.
 It is the procedure through which the quantity of the given test substance is
determined by the measured addition of titrant until the entire test substance
undergoes reaction. After the titration process, the potential difference between
the two electrodes (namely the reference and indicator electrode) is measured
in conditions where a thermodynamic equilibrium is maintained and the
current passing through the electrodes does not disturb this equilibrium.
ASSAY OF LEAD WITH POTASSIUM DICHROMATE SOLUTION
Procedure:
The amperometric titration may be carried out in a 100 ml beaker. A
saturated KNO3 salt bridge is employed to provide contact between the
saturated calomel electrode and the analyte solution.
1. Weigh accurately a sample of Pb-salt to give a 0.01 to 0.02 M lead solution
2. Transfer 10.0 ml aliquot to the titration vessel
3. Add to it 25 ml of the buffered supporting electrolyte, and 5 ml of the
gelatin solution
4. Determine the current at zero applied potential
5. Add K2Cr2O7 (0.01 M) solution, in 1 ml increments, and measuring the
resulting current
6. Continue the addition to at least 5.0 ml beyond the equivalence point
7. Correct the currents for the volume change, and plot the graph. Determine the
end-point and calculate the number of milligrams of Pb in the given sample
8. Repeat the titrations at – 1.0 V. It is essential to bubble N2 through the solution
for 10–15 minutes before the titration and while addition of reagents are made.
However, the flow of N2 must be stopped at the time of measuring the current.
Again, correct the currents for dilution, plot the graph, determine the end-point,
and report the number of milligrams of Pb present in the given sample.
Conductometric titration
Conductometric titration is a laboratory method of quantitative analysis used to
identify the concentration of a given analyte in a mixture. Conductometric titration
involves the continuous addition of a reactant to a reaction mixture and the
documentation of the corresponding change in the electrolytic conductivity of the
reaction mixture. In this type of titration, upon the continuous addition of the titrant
(and the continuous recording of the corresponding change in electrolytic
conductivity), a sudden change in the conductivity implies that the stoichiometric point
has been reached.
Applications of Potentiometric titration on pharmaceutical products:
1. Reproterol HCl and
2. Pipazethate HCl and
3. Salbutamol sulphate
References
 Journals:
 Direct potentiometry and potentiotitrimetry of warfarin and ibuprofen in pharmaceutical
preparations using PVC ferroin-based membrane sensors.
 Simultaneous determination of amoxycillin and clavulanic acid in pharmaceutical dosage
forms by LC with amperometric detection.
 Amperometric determination of dipyrone in pharmaceutical formulations with a flow cell
containing gold electrodes from recordable compact discs.
 Differential electrolytic potentiometric titration method for the determination of
ciprofloxacin in drug formulations.
 Thermodynamic dissociation constants of codeine, ethylmorphine and homatropine by
regression analysis of potentiometric titration data.
 British pharmacopeia 2009

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Different dosage with qualitative and quantitative analysis

  • 1. COURSE TITLE: PHARMACEUTICAL ANALYSIS IV COURSE NO: PHARM -4121 An Assignment on Different Dosage forms With their Quantitative and Qualitative Evaluation Submitted to: Dr. Md. Golam Hossain, Professor, Pharmacy Discipline, Khulna University Submitted by: Sk. Tanvir Raihan Emon 171111 Pharmacy Discipline Khulna University
  • 2. Dosage Form Dosage forms are pharmaceutical drug products in the form in which they are marketed for use , with a specific mixture of active ingredients and inactive components, in a particular configuration, and apportioned into a particular dose. For Example: Tablets, capsules , syrups etc.
  • 3. Types of Dosage Forms Depending on the physical form Solid Semisolid Liquid gaseous
  • 4. Types of Dosage Forms Depending on route of administration 1. Oral 2. Topical 3. Rectal 4. Vaginal 5. Parenteral 6. Inhaled 7. Optic 8. Opthalmic
  • 5. Oral Dosage Forms 1.Tablet: Tablet is a hard, compressed medication in round, oval or square shape. It mainly includes excipients such as binders, disintegrates, coating materials, sweeteners, disintegrates, glidants. For Example: Paracetamol Tablet, Antacid Tablet, Disprin Tablet
  • 6. Some subtypes of tablet 1. Compressed Tablet. Produced in large scale with a great pressure. Ex-Paracetamol 2. Coated Tablet. Has a covering over a tablet. Ex- Riboflavin 3. Buccal tablet. Administered by placing them in the mouth. Ex- Nitroglycerin 4. Effervescent Tablet. Designed to dissolve in water, and release carbon dioxide. Ex- Disprin 5. Chewable Tablet. Are chewed within the buccal cavity prior to swallowing. Ex- Antacid 6. Dental cone. Ex- Dental miror 7. Pastilles.
  • 7. Oral Dosage Forms 2. Capsules: Capsule is a medicine contained in a water-soluble gelatin shell.. The shell is used to protect the API from degradation due to any gastric materials. There are generally two types of capsules. For Example: Doxicap (Doxicycline capsules)
  • 8. Liquid Preparations 3. Gargles and mouth washes These are liquid preparations, mainly used to prevent oral or throat infections. Ex- Listerine mouth wash 4. Oral Suspension Oral suspensions are liquid solution where solid active ingredients remain suspended inside the vehicle of the container. This medication are needed to be shaken before use other wise the medications will settle down and the mixture will not be homogenous. Ex- Phenytoin suspensions.
  • 9. Topical Preparations 5. Ointments These are semi solid greasy preparations for application in skin , rectum, vagina or in nasal mucosa. Example: Clobetasol Propionate ointment. 6. Pastes These are mainly ointments with a high concentration of fine solid particles. Ex- 30% salicylic acid
  • 10. Parenteral Preparations 7. Intravenous It’s a liquid administered directly into the bloodstream via a vain. The solution must be sterile. The biggest advantage of IV preparations is that as there are no absorption phases, the drug is rapidly distributed to give quick action inside the body. Ex- Glucose preparations 8. Intramuscular It is the injection of a liquid directly into the muscle. Ex- Different vaccines are made as IM preparations, Like BCG vaccine. 9. Subcutaneous injection In this injection, the liquid is directly pushed into the cutis, the layer below dermis and epidermis of skin. Ex- Insulins
  • 11. 10. Ophthalmic preparations These medications are generally liquid or semi solid cream in nature and are intended for application to the conjunctiva or the eyelids. They are used to prevent eye infections and so must be sterile. Ex- Vaseline. 11. Rectal Preparations Rectal medicines are medications prepared specifically for insertion into the rectum. They are compounded in many forms. Among them the most popular and widely used are suppositories which are prepared by mixing medicine with a wax-like substance to form a semi-solid, bullet-shaped form that will melt after insertion into the rectum. Ex: Paracetamol suppositories
  • 12. Qualitative assay of different pharmaceutical dosage form
  • 13. Aciclovir Oral Suspension Assay Procedure: 1. To a weighed quantity containing 0.4 g of Aciclovir add 400 ml of water and 25 ml of 1M sulphuric acid , shake well, disperse with the aid of ultrasound for 10 minutes and add sufficient water to produce 500 ml. 2. Filter the resulting solution, discard the first few ml of filtrate and dilute 5 ml of the filtrate to 200 ml with 0.05M sulphuric acid . 3. Add 10 ml of the resulting solution to 5 ml of a 0.01% w/v solution of cetrimide in 0.05M sulphuric acid add sufficient 0.05M sulphuric acid to produce 100 ml and measure the fluorescence, Appendix II E, using an excitation wavelength of 308 nm and an emission wavelength of 415 nm.
  • 14. 4. Set the instrument to zero using a 0.0005% w/v solution of cetrimide in 0.05M sulphuric acid . 5. Calculate the content of C8H11N5O3 in the oral suspension from the fluorescence obtained by carrying out the operation at the same time using a mixture prepared by adding 10 ml of a 0.002% w/v solution of aciclovir BPCRS in 0.05M sulphuric acid and beginning at the words to 5 ml of a 0.01% w/v solution of cetrimide ...'. Determine the weight per ml of the oral suspension, Appendix V G and calculate the content of C8H11N5O3, weight in volume, using the declared content of C8H11N5O3 in aciclovir BPCRS . Source: Volume 3, page no:7919 (Brithish pharmacopeia 2009
  • 15. Benzoyl Peroxide Cream Assay Procedure: 1. Mix a quantity of the preparation being examined containing the equivalent of 0.25 g of anhydrous benzoyl peroxide with 50 ml of acetone and add sufficient acetone to produce 100 ml. 2. To 10 ml add 25 ml of a 20% w/v solution of potassium iodide , mix, stopper the flask and allow to stand for 15 minutes protected from light. 3. Add 25 ml of acetone and titrate with 0.01M sodium thiosulphate VS using starch mucilage , added towards the end of the titration, as indicator. 4. Repeat the operation without the substance being examined. The difference between the titrations represents the amount of sodium thiosulphate required. 5. Each ml of 0.01M sodium thiosulphate VS is equivalent to 1.211 mg of C14H10O4. Source: Volume 3, page no:8088 (British pharmacopeia 2009)
  • 16. Quantitative assay of different pharmaceutical dosage form
  • 17. Potentiometric Titration  Potentiometric titration is a laboratory method to determine the concentration of a given analyte. It is used in the characterization of acids. In this method, there is no use of a chemical indicator. Instead, the electric potential across the substance is measured.  It is the procedure through which the quantity of the given test substance is determined by the measured addition of titrant until the entire test substance undergoes reaction. After the titration process, the potential difference between the two electrodes (namely the reference and indicator electrode) is measured in conditions where a thermodynamic equilibrium is maintained and the current passing through the electrodes does not disturb this equilibrium.
  • 18. ASSAY OF LEAD WITH POTASSIUM DICHROMATE SOLUTION Procedure: The amperometric titration may be carried out in a 100 ml beaker. A saturated KNO3 salt bridge is employed to provide contact between the saturated calomel electrode and the analyte solution. 1. Weigh accurately a sample of Pb-salt to give a 0.01 to 0.02 M lead solution 2. Transfer 10.0 ml aliquot to the titration vessel 3. Add to it 25 ml of the buffered supporting electrolyte, and 5 ml of the gelatin solution 4. Determine the current at zero applied potential
  • 19. 5. Add K2Cr2O7 (0.01 M) solution, in 1 ml increments, and measuring the resulting current 6. Continue the addition to at least 5.0 ml beyond the equivalence point 7. Correct the currents for the volume change, and plot the graph. Determine the end-point and calculate the number of milligrams of Pb in the given sample 8. Repeat the titrations at – 1.0 V. It is essential to bubble N2 through the solution for 10–15 minutes before the titration and while addition of reagents are made. However, the flow of N2 must be stopped at the time of measuring the current. Again, correct the currents for dilution, plot the graph, determine the end-point, and report the number of milligrams of Pb present in the given sample.
  • 20. Conductometric titration Conductometric titration is a laboratory method of quantitative analysis used to identify the concentration of a given analyte in a mixture. Conductometric titration involves the continuous addition of a reactant to a reaction mixture and the documentation of the corresponding change in the electrolytic conductivity of the reaction mixture. In this type of titration, upon the continuous addition of the titrant (and the continuous recording of the corresponding change in electrolytic conductivity), a sudden change in the conductivity implies that the stoichiometric point has been reached. Applications of Potentiometric titration on pharmaceutical products: 1. Reproterol HCl and 2. Pipazethate HCl and 3. Salbutamol sulphate
  • 21. References  Journals:  Direct potentiometry and potentiotitrimetry of warfarin and ibuprofen in pharmaceutical preparations using PVC ferroin-based membrane sensors.  Simultaneous determination of amoxycillin and clavulanic acid in pharmaceutical dosage forms by LC with amperometric detection.  Amperometric determination of dipyrone in pharmaceutical formulations with a flow cell containing gold electrodes from recordable compact discs.  Differential electrolytic potentiometric titration method for the determination of ciprofloxacin in drug formulations.  Thermodynamic dissociation constants of codeine, ethylmorphine and homatropine by regression analysis of potentiometric titration data.  British pharmacopeia 2009