A very BIG thanks to you all lecturers. Thanks for yours inculcation within the year. =)

Assoc. Prof. Dr. Mohd Cairul Iqbal Mohd Amin

Deputy Dean of Undergraduate, Alumni & International

Dr. Mohd Hanif Zulfakar

Head for Drug Delivery Research Centre

Dr. Haliza Katas

Coordinator for Undergraduate Programme

Dr. Ng Shiow Fern

Coordinator for e-Learning

Practical 2 ; Sieving

TITLE: 

Sieving

OBJECTIVE :

1. To determine the particle size distribution of the powder materials and the size of solid particles by using the ‘sieve nest’ method.

INTRODUCTION:

                Sieving is the process of classifying powders by particle size distribution. The particle size distribution is defined via the mass or volume. Sieve analysis is used to divide the particulate material into size fractions and the weight of these fractions is determined. The most common media used in sieving is test sieves which are usually round frame, in sizes that range from 3 inches to 18 inches in diameter.

                 A sieve test is performed by first assembling a stack of interlocking sieves. The sieve with the largest openings is at the top and each lower sieve will have a smaller opening than the one above it. A pre-weighed sample of the material to be tested is placed in the top sieve. The sieve stack is shaken until all the materials has either been retained on a sieve or passed through. The material retained in each sieve is weighed and compared to the weight on the other sieves. A sieve test analysis or distribution is calculated which shows the proportion of each particle size category in the sample.

PROCEDURE:

1. 100g of lactose is weighed.
2. The ‘sieve nest’ in ascending order and provided appropriate sieve size is prepared.
3. Lactose powder is put into the sieve.
4. The powder is shaken or sieved in the sieve for about 20 minutes.
5. The results obtained are weighed and the graph of powder particle size distribution is plotted.
6. The process is repeated by using microcrystalline cellulose (MCC).

RESULT:

Sieving for lactose

Diameter of the test sieve (mm)	Amount of lactose obtained after sieving for about 20 minutes (g)
12	0.01600
10	0.02680
8	0.01580
6	30.5680
5	57.4950
3	11.1636

Sieving for microcrystalline cellulose (MCC)

Diameter of the test sieve (mm)	Amount of microcrystalline cellulose obtained after sieving for about 20 minutes (g)
12	0.00350
10	0.00430
8	0.07870
6	4.94850
5	51.8688
3	42.1931

DISCUSSION:

                In this experiment, a ‘sieve nest’ is used to determine the particle size distribution of 100g of lactose and microcrystalline cellulose. After being sieved for about 20 minutes, both lactose and microcrystalline cellulose obtained in each sieves with different diameters are weighed.

                 From the results obtained, it showed that there are small amount of powder obtained in sieve with diameter 12mm which are 0.001600g lactose and 0.000350g of microcrystalline cellulose. It means that the particle size of the powders is not under the range of that size or the powder particles are might be finer than that size. Observing and weighing the other sieves with increasing magnitude of fineness and limited, varying the amount of powder obtained. For lactose, it is said to have the particle size in range of 4mm to 5mm as there is high amount of lactose powder obtained in the sieve with diameter of 5mm which is 57.4950g. For microcrystalline cellulose, it have the same size range with lactose which is at range of 4mm to 5mm.This can be proven as the amount of MCC powder obtained in sieve with diameter 5mm is the highest comparing with other sieves which is about 51.8688g.

QUESTIONS:

1. What is the overall particle size of lactose and MCC?

                   Sieving is one of the oldest methods of classifying powders by particle size distribution. The nest of sieves is subjected to a standardized period of agitation, and then the weight of material retained on each sieve is accurately determined. The test gives the weight percentage of powder in each sieve size range. The selected sieves should be assembled with the coarsest sieve at the top of the stack and the balance of the stack in increasing magnitude of fineness which is increasing sieve numbers with smaller openings. The size parameter involved in determining particle size distributions by analytical sieving is the length of the side of the minimum square aperture through which the particle will pass.

                     Based on both graph plotted for sieving of lactose and MCC, it can be seen that most of both lactose and MCC particles are obtained in the sieve with 5 mm diameter. It indicated that both particles are about having small and finer size which can pass all the sieves with increasing magnitude of fineness and limited until the smallest opening of sieve which is 3 mm.

2. What are the other methods that can be used to evaluate the size of a particle?

                         Other method that can be used to evaluate the size of a particle is laser light scattering or LD technique. In this latter method, the forward diffraction of laser beam by particles is used to determine their size distribution. The angle of diffraction is inversely proportional to particle size, and the intensity of the diffracted beam at any angle is measure of the number of particles with a specific cross- sectional area in the beam’s path. Two optical models are commonly used to calculate the particle size distributions which are the Fraunhofer diffraction model and the Mie theory.

                          Main advantages of LD technique for particle size distribution determination include short time of analysis, high repeatability, small size of sample needed and a wide range of fractions into which the entire range of particle sizes can be divided.

                          The main disadvantages are high cost of LD instruments and insufficient confidence in the results due to the relatively low number of LD analyses of soils as compared with the enormous number of analyses performed by the classical methods.

3. What is the importance of particle size in a formulation?

The particle size distribution of active ingredients and excipients is the most important physical characteristics of materials especially in using them to create pharmaceutical products. The size, distribution and shape of the particles can affect the bulk properties, product performance, process ability, stability and appearance of the end product. The relationship between particle size and product performance is well influenced to the dissolution, absorption rates and content uniformity. Particle size analysis is also important in order to formulate and manufacture many pharmaceutical dosage forms.

CONCLUSION:

                      In conclusion, by using ‘sieve nest’ method, the particle size distribution and size of solid particles of both powders used in this experiment which are lactose and microcrystalline cellulose is in range of 4mm to 5mm.

REFERENCE:

1. http://www.newdruginfo.com/pharmacopeia/usp28/v28230/usp28nf23s0_c786.htm
2. http://www.cscscientific.com/particle-size/sieves/

Practical 1; Ball Milling

Title: 

Ball Milling

Objectives:

1. To study the technique of using ball mill.
2. To determine the distribution of the particle sizes.
3. To study the factors affect the milling process.

Introduction:

                     Grinding or milling is a process to break the solid material into smaller pieces or even into powder. It is widely used in industrial to obtain desired size of the product. The size of the product depends solely on the time of grinding and the speed of the grinder.

                      In our experiment, a device known as ball mill will be used. Ball mill is a type of the grinder which is cylindrical in shape and the cylinder is a hollow cylinder. It rotates around a horizontal axis and partially filled with the media and the material to be ground. The materials of the media are stainless steel balls. It follows the theory of combined impact and attrition methods.

                     During the rotation, the metal balls will be raised up and fall back to the base in the hollow cylinder. This will produce a cascading action to crunch the medium in the cylinder. Therefore, the desired sizes of the particles are produced.

                      Sieving is one of the methods to determine the particle sizes. The device used in sieving is sieve. Sieve contains known sieve diameter of small holes whereby it allows the particles to pass through the holes. By doing this, we are able to obtain the particles with known range of sizes.

                       In our experiment, a stack of sieves will be used. The ranges of the sieve that we used were 150µm, 250µm, 300µm and 500µm.

Chemicals and Apparatus:

Coarse salt

Ball mill
Sieve
Electronic balance

Methods:

1. 369.3g of coarse salts were weighted by using electronic balance.
2. Same number of same size metal balls was put into the hollow cylinder of the mill.
3. Then, the coarse salts were filled into the hollow cylinder of the mill.
4. The “milling” process is begun for 10 minutes with the speed of 5.
5. The product was obtained and weighted again to check the amount of the salts.
6. Next, the fine particles were put into the sieve for sieving.
7. After that, the fine particles from each sieve net were collected for weighing purpose.
8. Lastly, a graph (histogram) was plotted by using the weight of the obtained fine particles.

Results:

Weight of salt before milling = 369.3g
Weight of salt after milling = 358.5g 

Discussion:

                        In our experiments, we found out that there are 2 factors that influence the particles size during the milling process. First factor is the time of grinding. It is found out that the longer the time of grinding, the more the finest particles we can obtain. This is because longer time frame of grinding allows more collision of the particles with the metal balls. Therefore, higher time frame of rotation allows more finest particles to be obtained. This statement is shown in the data of group 5&6 and group 7&8 whereby group 7&8 contains more finest particles (0.4682g of particles in the range of 150µm < x ≤ 250µm) compare to group 5&6 (0.2967g). Both of these groups used the same rotating speed but different time frame of grinding. Group 5&6 carried out their experiment for 10 minutes but group 7&8 carried out their experiment for 20minutes. Therefore, group 7&8 obtained more finest particles.

                     When we compared the data from group 1&2 and group 3&4, we found out that group 1&2 has more finest particles (5.0079g) compare to group 3&4 (2.8825g). This is not following the correct manner because group 1&2 and group 3&4 carried out their experiment with the same speed but different time frame whereby group 1&2 carried out their experiment in a shorter time compare to group 3&4. The amount of finest particles collected by group 1&2 should be lesser than group 3&4. This usual of data may due to errors occurred throughout the experiment. One of the most common errors that might occur was the speed of agitation during sieving. Group 3&4 might not agitated the sieve properly and caused most of the finest particles stayed in the top sieve net. Besides, group 3&4 might not put in the same number of metal balls into the hollow cylinder as other groups. This caused the milling process did not reach the optimal level and leave out a lot of large particles.

                     The second factor that may influence the result of the data is the speed of the rotating cylinder. It is found out that higher speed of rotation will result in higher production of finest particles. At low angular velocities, the metal balls move with the drum until the force due to the gravity exceeds the frictional force of the bed on the drum, and the balls then slide back to the bed of the drum. Instead, at higher angular velocities, a motion known as cascade will be produce whereby the metal balls are lifted up until their dynamic angle of repose is exceeds, they will fall back to the bed of the drum in a cascade across the diameter of the cylinder. This allows the maximum size reduction. In the data that we had collected, we supported the theory. Group 1&2 and group 5&6 used the same time frame of rotation but different speed of rotation whereby group 1&2 used higher angular velocities to carry out the experiment. Therefore, group 1&2 able to collect more finest particles compared to group 5&6.

                      In our experiment, we found out that group 3&4 contained the most amount of large particles compared to the rest of the group. This unusual data may because the cylinder moved at high speed with less amounts of metal balls inside and the balls are thrown out of the mill (cylinder) wall by centrifugal force and caused less size reduction of the materials. Therefore, it was found out that group 3&4 had the highest amount of large particle due to incomplete milling process.

                       In our experiment, we used the ball mill as the grinder to reduce the particle size. Ball mill uses combined impact and attrition methods. Besides the ball mill that we used, there are several other devices can be used to reduce the size. There are cutter mill, hammer mill, vibration mill, roller mill and fluid energy mill.

                        Cutter mill is an equipment that used the principal of cutting method whereby it able to produce the particle size from the range of 100µm up to 100 000µm. Next, hammer mill is a device that uses the principal of impaction. Hammer mill able to produce the particle size from the range of less than 10µm up to nearly 100 00µm. Vibration mill also uses the principal of impaction but it is different from the regular hammer mill whereby it is filled with steel ball and vibration of whole mill will occur. During the vibration, impaction between the steel balls and the materials will reduce the materials into small particles.

                         There is a device known as roller mill where it uses the principal of attrition to produce size reduction of solids in suspensions, pastes or ointments. This roller mill can produce the particle as small as 20µm. Fluid energy mill is a device that had the same principal as the ball mill as mentioned above. The high kinetic energy of the air of the fluid energy mill causes the particle to impact with other particles and fracture occurs. These fractures break the particles into smaller size.

                         There are few factors needed to be aware when we want to select the correct device for the reduction of particle size. One of the factors is the shape of the particles that we wanted to produce. Besides, we must know that each device will give different size of the final particles. Therefore, we must know the particle size that we are required before we select the correct device. Next, the surface hardness of the material should be considered before the selection of the equipment as the surface hardness may varies the particle size. The surface hardness can be determined by using the Mohs’ scale.

Conclusion:

                         From our experiment, we learnt how to setup the ball mill and we were able to use it correctly throughout the experiment. Besides, we found out that most of the fine particles were produced with higher speed or longer time frame of the grinding process. Therefore, we conclude that angular velocity of the ball mill and the time of grinding process affects directly to the particle size. Angular velocity of the ball mill inversely proportional to the particle size yet the particle size will remain unchanged if the angular velocity is too high. Instead, the time frame of grinding is inversely proportional to the particle size.

References: 

1. M.E.Aulton. 2004. Pharmaceutics, The Science of Dosage Form Design 2nd Ed. Churchill livingstone. Pg 166 – 173

Experiment 3 ; Uniformity of weight of tablets and capsules.

Title: 

Uniformity of weight of tablets and capsules.

Objective: 

To determine whether the uniformity of weight of tablets and capsules studied comply with the standard of British Pharmacopoeia or not.

Introduction:

                   Uniformity of weight of drug is important because this ensure the even distribution of ingredients in the drug. Uneven distribution may alter the dose in each individual drug and therefore causes a lot of problems such as unable to reach the therapeutic range or exceed the therapeutic range and reach toxic range.

                   In our experiment, we determined the weight of the tablets and capsules. Next, we determined the deviation percentage of each tablet and capsule that weighted. By doing this, we able to determine the uniformity of weight of tablets and capsules studies that comply with the standard of British Pharmacopoeia or not

Materials and apparatus:

Tablet : Uphamol
Capsule : Ampicillin

Weighing balance

Methods:

Tablets

1. 20 tablets previously selected at random were weighed. The average weight was determined.
2. The tablets were weighed individually and for each tablet , the percentage deviation of its weight from the average weight was determined.
3. The deviation of individual weight from the average weight should not exceed the limits given below. 

Capsules

1. 20 capsules were selected randomly.
2. One of the capsules was weight. Then, the capsule was opened and its contents were removed completely before next step.
3. Next, the weight of the capsule was weight and net weight of the contents was determined.
4. The same procedures were repeated for other 19 capsules.
5. The average net weight was then determined by sum up all the individual net weights.
6. The percentage deviations of the tablets’ weight were determined.
7. The deviation of individual net weight should not exceed the limits given below.

Results and Calculations:


Tablets :

Capsules :

Discussion: 

                        According to the results obtained, the average weight of the tablet Uphamol is 0.6446 g (644.6mg). This indicates that the Uphamol tablets are at the range of more than 250mg. Therefore, this tablet should has minimum 18 tablets that in the range of ± 5.0% and maximum 2 tables that in the range of ± 10.0%. For the data we obtained, it is found out that all the tablets follow the limits given. 18 of the tablets are in the range of ± 5.0% and 2 of the tablets are in the range of ± 10.0%. The maximum deviation percentage is -5.5538%. This shows that all tablets used is our experiment are uniform from the aspect of weight.

                       The average weight of the capsule Amipicilin is 0.3741g (374.1mg). Therefore, this capsule should has minimum 18 capsules that in the range of ± 7.5% and maximum 2 capsules that in the range of ± 15.0%. For the data we obtained, it is found out that all the capsules follow the limits given. 20 of the capsules are in the range of ± 7.5% and none of the capsules are in the range of ± 15.0%. The maximum deviation percentage is -7.3138%. This shows that all capsules used is our experiment are uniform from the aspect of weight.

                          The errors might arise when measuring the weight of these tablets and capsules. Some powders might still get stuck inside the capsule shells and the powders are not completely removed, thus cause the measurement of emptied shells not accurate. Besides that, errors might also due to the air flow or wind around the weighing balance. All these errors will lead to inaccuracies of measurement of weight.

Conclusion: 

The uniformity of weight of tablets and capsules test are useful in quality control during the production of tablets and capsules. In this experiment, it is found that all tablets and capsules used are uniform.

Experiment 2 ; Tablet Friability

Title:

Tablet Friability

Objective:

I. To determine physical strength of uncoated tablets upon exposure to mechanical shock and attrition
II. To determine the percentage loss of weight of the tablet after being put into friabilator

Introduction:

                        Friability is the ability of a solid substance to be reduced to smaller pieces with little effort. In pharmaceutical, friability is the tendency for a tablet to chip, crumble or break following compression. This tendency is normally confined to uncoated tablets and surfaces during handling or subsequent storage. Friction and shock are the forces that most often cause tablets to chip, cap or break. The friability test is closely related to tablet hardness and is designed to evaluate the ability of the tablet to withstand abrasion in packaging, handling and shipping. The loss due to abrasion is a measure of the tablet friability. The value is expressed as a percentage. A maximum weight loss of not more than 1% of the weight of the tablets being tested during the friability test is considered generally acceptable and any broken or smashed tablets are not picked up. Normally, when capping occurs, friability values are not calculated. A thick tablet may have less tendency to cap whereas thin tablets of large diameter often show extensive capping, thus indicating that tablets with greater thickness have reduced internal stress

Procedure:

1. 10 tablets of ettrocin are selected and weighed.

2. All the tablets are put into the drum of tablet abration and friability tester. The rate of rotation is set to 25 rpm, time to 10 minutes, and the operation is started.

3. At the end of the operation, all the tablets is removed and ensured freedom from dust or powder (by using brush). The tablets are reweighed and the percentage loss of weight is determined.

4. The tablets should not lose more than 1% of its weight.

Results:

Initial weight of all tablets = 6.5966 g

Final weight of all tablets = 6.5426 g

% loss of weight = (6.5966-6.5426) X 100 %
6.5966
= 0.82 %

Discussion:

                     In friability test the tablets are prone to abrasion hence enabling us to check for the tablet strength under application of force in different manner. It can be caused by a number of factors including poor tablet design (too sharp edges), low moisture content and insufficient binder. For obvious reasons, tablets need to be hard enough such that they do not break up in the bottle but friable enough that they disintegrate in the gastrointestinal tract. Tablets prone to capping during the test are considered unfit for commercial use. Friability is affected by various external and internal factors like the punches that are in poor condition or worn at their surface edges, resulting in 'whiskering' at the tablet edge and show higher than normal friability values. Friability test is influenced by internal factors like the moisture content of tablet granules and finished tablets. Moisture at low and acceptable level acts as a binder. In this experiment, the percentage loss of weight of the tablets is 0.82 % which is not exceeding 1 %, the non-pharmacopeia standard. It shows that the tablets are quite able to resist mechanical shock and aberration during the test.

Conclusion:

The percentage loss of weight of the tablets is 0.82 %. Conventional compressed tablets that lose less than 0.5% to 1% of weight are considered acceptable and fit for commercial use.

References:

1. http://www.pharmainfo.net/tablet-evaluation-tests/mechanical-strength-tablets/friability
2. http://www.anabiotec.com/testing/detail/hardness-friability-disintegration
3. http://www.who.int/medicines/publications/pharmacopoeia/TabletFriability_QAS11-414_FINAL_MODIFIED_March2012.pdf

Experiment 4 ; Dosage Performance Tests

Title :

Dosage Performance Tests

Introduction :

                         Tablet is defined as a compressed unit solid dosage form containing medicaments with or without excipients. According to Indian Pharmacopoeia, pharmaceutical tablets are solid, flat or biconvex dishes, unit dosage form, prepared by compressing a drugs or a mixture of drugs, with or without diluents. Sugarcoat protects the enclosed drug from the environment and provides a barrier to objectionable taste or order. The sugar coat also enhances the appearance of the compressed tablet and permit imprinting manufacturing’s information. Sugar coating provides a combination of insulation, taste masking, smoothing the tablet core, colouring and modified release.

                          Disintegrating agent is always added to tablet formulation to facilitate its breaking when it contact with water in gastrointestinal tract. It’s aim is to increase the surface area of the tablet fragments and thus promote release of the drug. A good disintegrant will quickly break up a tablet into primarily particles and ensure that the drug is assimilated at a fast rate. Disintegrants act by swelling in the presence of water to burst open the tablet. Starch is the most common disintegrant in tablet formulation. Example of starch derivatives are Primogel and Explotab. Other common disintegrants include cation exchange resins, cross-linked polyvinylpyrrolidone, modified starches (sodium starch glycollate) and cellulose materials. Superdisintegrants swells up to ten fold within 30 seconds when contact water. Examples include Crosscarmellose and Crosspovidone. Evaluation of carbon dioxide in effervescent tablets is also one way of tablet disintegration.

                        Whereas dissolution or solvation is the process by which a solute forms a solution in a solvent. The solute, in the case of solids, has its crystalline structure disintegrated as separate ions, atoms, and molecules form. The outcome of the process of dissolution which is the amount dissolved at equilibrium, is governed by the thermodynamic energies involved, such as the heat of solution and entropy of solution, but the dissolution itself (a kinetic process) is not. Dissolution testing has emerged in the pharmaceutical field as a very important tool to characterize drug product performance. In formulation development, dissolution testing can aid in the selection of excipients and help optimize the manufacturing process, The significance of a dissolution test is based on the fact that for a drug to be absorbed and available to the systemic circulation, it must previously be dissolved Therefore, dissolution tests are used not only for quality control of finished products, but also to assess several stages of formulation development, for screening and proper assessment of different formulations.

Procedures :

Disintegration test for sugar-coated tablets

1. The apparatus is set up for the disintegration test according to it’s operation manual.

2. The temperature of the disintegration medium (water) is ensured at 37+2’C.

3. The time is set to 60 minutes. One tablet is introduced into each tube, the disk is added into each tube and start the operation.

4. The tablet in each tube is checked at the end of the operation.

5. If all 6 tablets disintegrate in 60 minutes, then tablets comply with the test. If there is any tablet that does not disintegrate, the test is repeated using 6 new tablets but the disintegration medium (water) is replaced with 0.1M hydrochloric acid. Tablets comply with the test if all 6 tablets disintegrate in the acidic medium.

Dissolution test for tablets

1. Each of the dissolution vessel is filled up with the buffer solution to 900ml mark. The temperature is set to 37’C.

2. Temperature of the dissolution medium is checked and ensured it is at 37+0.5’C.

3. One Ibuprofen Tablet is placed into each dry basket assembly.

4. The stirring speed is set to 150rpm. The basket assembly is lowered into position in the vessel and operation is started.

5. 10ml samples of the dissolution medium is withdrawed from each vessel after 30 minutes for analysis and the solution is filtered using suitable filter. Sampling should be done from a point half-way between the surface of the dissolution medium and the top of the rotating basket, and not less than 10mm from the wall of vessel. The volume of aliquot withdrawn for analysis is replaced with an equal volume of same dissolution medium.

6. A standard solution of ibuprofen is prepared by diluting 10.0mg of ibuprofen reference standard to 50ml with dissolution medium.

7. 2.0ml of sample solution and 2.0ml of standard solution to 25ml is diluted with dissolution medium in separate volumetric flasks.

8. The absorption of both solutions is measured in a 1cm cell at a wavelength of 2.21nm.

9. The percentage amount of ibuprofen dissolved using the following formula is calculated：　

                  At/As x W/50 x 2/25 x P x 900 x 25/2 x 100/200

Where At = absorbance of sample solution

           As = absorbance of the standard solution
           W = weight of ibuprofen reference standard used
            P = purity of ibuprofen reference standard

10. Whether the tablets comply with the requirements of the United States Pharmacopoeia is determined from the results obtained.
USP limits : Not less than 75% of the stated amount of C13H18)2 dissolved in 30 minutes.

Results and Calculations:

Disintegration test for sugar-coated tablets

Table 4.1 Disintegration times for the sugar-coated tablets in 37’C water bath
The result is 4.77minutes for the 3 tablets to fully disintegrate. The drug used is NSAID.

Dissolution test for tablets

     At/As x W/50 x 2/25 x P x 900 x 25/2 x 100/200

At = absorbance of sample solution
As = absorbance of the standard solution
W = weight of ibuprofen reference standard used
P = purity of ibuprofen reference standard

As a calculation:

At=0.5182, As=0.4988, W=10 grams, P=0.98

0.5182/0.4988 x 10/50 x 2/25 x 0.98 x 900 x 25/2 x 100/200
=84.90%

Discussion:

                    Coated tablets are tablets covered with one or more layers of mixtures of substances such as natural or synthetic resins, polymers, gums, fillers, sugars, plasticizers, polyols, waxes, colouring matters and many more. Sugar-coated tablets we used in ecperiment, Ibuprofen comply with Disintegration test for tablet. The specification test state that all of the coated tablets should disintegrate within 15 minutes. The end point was determined when there were no particles or granules remaining in the discs. The average disintegration time for 3 tablets are 8.77 minutes which shown in table 4.1. Three of the tablets are of same brand, so they have similar disintegration time. Ibuprofen is a propionic acid derivative that belong to the class NSAID. Disintegration result show that Ibuprofen tablets developed resistance to strong acid. Thus, it will not disintegrated in stomach, preventing complications like gastric pain.

                    Dissolution test is to measure the amount of active ingredient the has dissolved in a volume of dissolution medium at the prescribed time, using an apparatus specially designed according to the experimental parameters. It is the amount (percentage) that must be dissolve in time (minutes).For dissolution test for tablet, the percentage amount of ibuprofen dissolved are 84.90%. This show that the tablet comply with the requirement of the United States Pharmacopoeia (not less 75% of the stated amount of C13H18O2 dissolved in 30 minutes.

Conclusion :
                      As a conclusion, disintegration test is used in the pharmaceutical industry for evalution of disintegration capability of formulations (ex:tablets) and quality control of different dosage forms. Dissolution test is one of the most important quality control tests performed on pharmaceutical dosage forms and is now developing into a tool for predicting bioavailability, and in some cases, replacing clinical studies to determine bioequivalence. Dissolution behavior of drugs has a significant effect on their pharmacological activity.

References :

1. Aletaha, D.; Smolen, J. S. Advances in anti-inflammatory therapy. Acta Medica Austriaca., v.29, n.1,        p.1-6, 2002.
2. http://www.pharmainfo.net/tablet-evaluation-tests/dissolution
3. http://www.pharmainfo.net/disintegration-test

ASSESSMENT OF QUALITY OF TABLET AND CAPSULE

ASSESSMENT OF QUALITY OF TABLET AND CAPSULE

INTRODUCTION:

            Tablets and capsules are parts of many type of dosage forms. Liquid dosage forms such as syrups, suspensions, emulsions, solutions and elixirs usually contain one dose of medication in 5 to 30 ml. the oral route administration is the most important method for systemic effects. In topical route administration, which has been employed with nitro-glycerine for the treatment of angina and scopolamine for motion sickness, there would be effective drug absorption for systemic drug action of drugs that are administered orally. This can be represent by the solid oral dosage forms such as tablets and capsules which are the most preferred class of products of two forms as tablet has many advantages. One of the advantages is tablet is an essentially tamper proof dosage form.

           The standard quality control tests such as diameter, size and shape, uniformity of weight, thickness, hardness, friability, percentage of medication (assay), rate of disintegration, dissolution and solubility can be carried out on compressed tablets for their evaluation. The aim of these evaluations is to study the effect of composition of formulations in drug release rate.

            Tablet diameter is an important test that has to be carried out. Tablet thickness can be measured by micrometer or by other device.  The thickness of the tablet should be controlled within a ± 5% variation of standard value. Hardness can be defined as the strength of the tablet to withstand the pressure applied. The hardness of the tablet depends on the weight of the material used, space between the upper and lower punches at the time of compression and pressure applied during compression. It is also depends on the nature and quantity of recipients used during formulation. Tablet thickness is important in tablet packaging. Tablet that is very thick will affects the packaging either in blister or plastic container.

            Friability test can be performed to evaluate the ability of the tablets to withstand abrasion in packing, handling and transporting. To examine this, tablets are subjected to a uniform tumbling motion for specified time and weight loss is measured. The breakage of tablet into smaller fragments is called disintegration of tablet. The dissolution test represent the release of drug from tablet into solution per unit time under standardize condition. The disintegration testing is used as surrogate for the dissolution of solid oral dosage forms, since it is recognized that the disintegration into smaller particles is essential for the absorption by the body.

There are five experiment in this assessment ;

1.Uniformity of diameter, thickness and hardness

2. Tablet friability

3.Uniformity of weight of tablets and capsules

4. Dosage performance test

5. Content of ibuprofen

Experiment 1 ; Uniformity test of diameter,thickness and hardness

EXPERIMENT 1: 

Uniformity test of diameter,thickness and hardness.

OBJECTIVE:

1.      To determine the uniformity of tablets in diameter, thickness and hardness.

PROCEDURE:

10 tablets are chosen and examined using Tablet Testing Instrument, PTB 311 (PHARMATEST) for their uniformity in diameter, thickness and hardness. The deviation of individual unit from the mean diameter is calculated and ensured to not exceeding ± 5% for tablets with diameter of less than 12.5 and ± 3% for diameter of 12.5 mm or more. 

RESULTS:

TABLET	DIAMETER (mm)	THICKNESS (mm)	HARDNESS
1	13.13	5.49	113.9
2	13.16	5.46	108.4
3	13.16	5.50	131.1
4	13.13	5.50	128.3
5	13.11	5.49	116.6
6	13.18	5.50	115.3
7	13.13	5.45	112.2
8	13.12	5.50	100.1
9	13.14	5.47	102.2
10	13.13	5.47	110.5

CALCULATION:

Mean of diameter (mm) = Total diameter of all tablets / 10

 = (13.13 + 13.16 + 13.16 + 13.13 + 13.11 + 13.18 + 13.13 + 13.12 + 13.14 + 13.13) / 10

   = 13.139 mm

Percentage (%) = │ (Experimental diameter – Mean diameter) / Mean diameter│ X 100

TABLET	PERCENTAGE (%)
1	0.0685
2	0.1598
3	0.1598
4	0.0685
5	0.2207
6	0.3120
7	0.0685
8	0.1446
9	0.0076
10	0.0685

DISCUSSION:

                    In this experiment, 10 tablets of the same type are used to test their uniformity in diameter, thickness and hardness. From the results obtained, it showed that the diameter and thickness of each tablet are slightly same comparing to each other. The diameter of the tablets is at range of 13.13 mm to 13.18 mm whereas the thickness of the tablets is at range of 5.45 mm to 5.50 mm. This indicates that the tablets have achieved the uniformity in diameters and thickness. For the hardness of each tablets, the result obtained proved that one tablet will have its own hardness which is it might be same or different to other tablets. Commonly, the hardness of the individual tablet will be slightly different compared to others.

                  The uniformity of diameter of the tablets can be further proven with the percentage difference that has been calculated. Theoretically, tablets with diameter 12.5 mm or more than 12.5 mm would have not more than 3% of individual deviation from the average diameter. From the results obtained, it showed that all the tablets have achieved percentage difference below than 3%. This means that each tablets had obey the theoretical value of standard diameter.

CONCLUSION:
                     Tablets with the same type are commonly have slightly similar or uniform value in their diameter and thickness. However, it has distinct value in measuring their harness as one unit of tablet has different hardness compared to other tablets. In conclusion, the uniformity of tablets in diameter, thickness and hardness are important in assessment of quality of tablets.

REFERENCES:

1. http://hussain-ku.blogspot.com/2010/11/quality-control-tests-for-tablets.html
2. http://www.sadgurupublications.com/ContentPaper/2012/4_133_JCCPS_2(1)2012_P.pdf
3. http://books.google.com.my/books?id=KorasAtSpfoC&pg=PA4&lpg=PA4&dq=performance+test+doses+(disintegration+and+dissolution)&source=bl&ots=A2677PXCjn&sig=NBlcIE3dg6e7hsbOiwjXTedPKsY&hl=en&sa=X&ei=NgW0Uv-dCofzrQflwICwDw&ved=0CGQQ6AEwBA#v=onepage&q=performance%20test%20doses%20(disintegration%20and%20dissolution)&f=false