PRACTICAL 3 : Experiment 4 - Dosage Performance Tests

Disintegration test for sugar-coated tablets

Procedure:

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

       2.      The temperature of the disintegration medium (water) was ensured at 37±2°C.

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

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

       5.      The Antibiotic tablet was complied with the test if it is disintegrate in 60 minutes. If there is any Antibiotic tablet that does not disintegrate, the test was repeated using the same tablet but the              disintegration medium (water) was replaced with 0.1M hydrochloric acid. The Antibiotic tablet          was complied with the test if it is disintegrate in the acidic medium.

Results:

Tablets	Disintegration test with water	Time needed to fully disintegrate
1	Pass	2.23 minutes

Discussion:

Disintegration test is only applicable for uncoated tablets, sugar coated tablets , enteric-coated tablets, soluble tablets, dispersible tablets, hard capsules, soft capsules and enteric capsules. Antibiotic tablet, which was used in this experiment, is a sugar coated tablets.

From this test, in average, an Antibiotic tablet would need 2.23 minutes to be fully disintegrate using Apparatus A setup. The standard set for this experiment was to have the tablet disintegrate not more than one hour in water medium. So, Antibiotic tablet have succeeded this test. But this results did not really imitate how the preparation would disintegrate in human body. Multiple parameters to really imitate our body system upon drug intake were not provided. Some of these parameters include the different pH and motility in different parts of gastrointestinal tract. This result is not guarantee to be the same as in an actual person. It might be lot more faster since the motility of human GI tract were quite vigorous and the pH were lower.  There might be preparation that failed this test but actually would be able to be fully disintegrate in an actual human. Still, this result is still come in handy in preformulation test so to reduce drug candidates thus to save time and money.

Some precaution need to be taken during this experiment.  The coating of a tablet did not subjected to be disintegrate within the time limit. We must pay close attention on identifying that the content of the tablet comply with the standard stated. When a formulation have reached the time limit but still have bit of it that did not fully disintegrate, check by squishing it to see whether the fragments still have part that did not come in contact with the water (still in it dry hard tablet or dry powdered tablet form). If the first batch did not meet the requirement, the test need to be repeated using same number of new tablet but the medium now is 0.1M hydrochloric acid. Usually, preparation that must succeed dissolution test did not have to do this test.

Conclusion:

     All Antibiotic tablets succeeded this test with the first tablet disintegrate in 2.23 minutes. This disintegration duration might not be the same as in real human body. Most likely, it would need shorter time due to more harsh condition (compared to subjected condition in the experiment).

Dissolution test for tablets

Procedure:

1.      The dissolution vessel was filled up with the buffer solution to 900 ml mark. The temperature was set to 37°C.

2.      The temperature of the dissolution medium was checked. It was ensured at 37±0.5°C.

3.      One Ibuprofen Tablet of 200 mg was placed into each dry basket assembly.

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

5.      After 30 minutes, 10 ml samples of the dissolution medium were withdrawn from each vessel for analysis and the solution was filtered using suitable filter. The sampling was taken out from a point half-way between the surface of the dissolution medium and the top of the rotating basket, and not less than 10 mm from the wall of the vessel. The volume of aliquot withdrawn was replaced for analysis with an equal volume of same dissolution medium.

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

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

8.      The absorption of both solutions was measured in a 1 cm cell at a wavelength of 221 nm.

Results:

Type of solution	Spectrophotometer absorbance reading
Standard	3.1351
Sample	0.7552

% amount of ibuprofen dissolved

= 0.7552/3.1351 x 10mg/50 x 2/25 x 0.98 x 900 x 25/2 x 100/200

=21.25%

·         The ibuprofen tablet is not complied  with the USP requirements

Discussion:

The reading of spectrophotometer for standard solution and sample solution are 3.1351 and 0.7752 respectively. Based on the result, the percentage amount of ibuprofen dissolved is 21.25%.

Thus, we can conclude that this tablet is not complied with the requirements United States Pharcomacopoiea as the percentage must be more than 75% to be approved as the complied one.

There may be several errors those have been made during the experiment is being conducted. The dissolution process of ibuprofen tablet could be incomplete thus, the spectrophotometer reading may be altered as spectrophotometer. Besides, the sample solution is not filtered by using the filter when the solution is being transferred into the volumetric flask. Thus, the small, undissolved ibuprofen tablets are also present in the volumetric flask. This will result in wrong reading of absorbance by the spectrophotometer due to the wrong concentration of the solution. This is because the amount of light absorbed by the solution is proportional to the concentration of the solute (ibuprofen) present.

Furthermore, the result obtained are not complied with the USP requirements maybe due to the expired tablet. An expired tablet will have a change in physicochemical properties including in the dissolution aspect thus resulting in incorrect result. The tablet must be rechecked and new batch should be produced to be tested again.

The parallax error also may occur during the reading of solution in the measuring cylinder and volumetric flask. The incorrect volume of both solution will alter the concentration of the solution, thus result in wrong reading of absorption in spectrophothometer. In order to overcome this problem, the experimenter must make sure that his eyes are perpendicular to the plane of measuring cylinder and the calibration mark of volumetric flask.

Conclusion:

From the experiment, the tested ibuprofen tablet is not complied with the USP requirements as only 21.25% of the tablet dissolved during the experiment.