Tablets and capsules represent unit dosage forms whereas liquid oral dosage forms such as syrups, suspensions, emulsions, solutions and elixirs usually contain one dose of medication in 5 to 30 mL. Such doses are erratic by a factor ranging from 20 to 50% when the drug is self administered by the patient.The oral route of drug administration is the most important method for systemic effects.
The standard quality control tests such as diameter, size and shape, uniformity of weight, thickness, hardness, friability, percentage of medicament (Assay), rate of disintegration, dissolution and solubility can be carried out on compressed tablets for their evaluation.
Experiment 1 Uniformity of diameter, thickness and hardness
Aim
:
1.
To test the uniformity of hardness,dimater and thickness for 10 samples of
tablet.
2.
to test the ablity for tablet to withstand sufficient mechanical strength and
fracture/erosion
during manufacturing and handling
3.
To enhance the patient compliance to drug with attractive appearance and suitable
hardness
Introduction
:
This
is important to facilitate packaging and decide tablet compressing machine to
use.
The
weight uniformity and content uniformity to make sure the correct dosage and
content of
drug.
Next, its concerned with sampling,testing and documentation during
manufacturing and
also
completion of manufacturing.
Procedure
:
1.
10 tablet of paracetamol is chosen and test for hardness,diameter and thickness
by using
tablet testing instrument.
2. The standard deviation of diameter not
more/less than 3% for tablet with diamater more
than and equal 12.5 mm and 5% for tablet 12.5 mm.
than and equal 12.5 mm and 5% for tablet 12.5 mm.
Result
:
Thickness
( mm ) |
Diameter
( mm ) |
Hardness
( N ) |
Standard Deviation (Thickness)
|
Standard Deviation (diameter)
|
Standard Deviation (hardness)
|
|
1.
|
5.500
|
13.130
|
112.900
|
- 0.040
|
- 0.024
|
+ 0.110
|
2.
|
5.500
|
13.130
|
113.900
|
- 0.040
|
- 0.024
|
- 0.890
|
3.
|
5.440
|
13.130
|
113.900
|
0.020
|
- 0.024
|
- 0.890
|
4.
|
5.470
|
13.120
|
103.600
|
- 0.010
|
- 0.014
|
- 0.600
|
5.
|
5.450
|
13.110
|
89.800
|
0.010
|
- 0.004
|
+ 23.210
|
6.
|
5.500
|
13.110
|
144.200
|
- 0.040
|
- 0.004
|
- 31.190
|
7.
|
5.480
|
13.120
|
118.000
|
- 0.020
|
- 0.014
|
- 4.990
|
8.
|
5.500
|
13.110
|
126.600
|
- 0.040
|
- 0.004
|
- 13.590
|
9.
|
5.500
|
13.130
|
117.000
|
- 0.040
|
- 0.024
|
- 3.990
|
10.
|
5.280
|
12.970
|
109.800
|
- 0.180
|
+ 0.136
|
+ 3.210
|
Average : 5.460
|
13.106
|
113.010
|
||||
Average
of hardness : 5.460 mm
( 5.500 + 5.500 + 5.440 +
5.470 + 5.450 + 5.500 + 5.480 + 5.500 + 5.500 + 5.2
80 )
80 )
10 samples
Average
of diameter : 13.106 mm
10 samples
Average
of Hardness : 113.010 N
(112.900 + 113.900
+113.900 + 103.600 + 89.800 + 144.200 + 118.000 + 126.600 + 117.000 + 109.800 )
10 samples
10 samples
Discussion
:
1.Thickness :
Most
common range of thickness for paracetamol tablet from samples is 5.28 mm till
5.50 mm.Theoretically in market the dosage range start with 5.76 mm till 5.97
mm but it is depend on the dosage given.
The
standard deviation from the table show limit for tablet to be released to
market must be not more and less than 5 % (0.273 mm).The experiment is accepted
since the thickness within range between - 0.040 till - 0.180. The thickness
uniformity essential for packaging and dosage range.It also to prevent the
patient think the big and thick size of tablet means have a best dosage so
reduce from 2 times a day to 1 times a day.
The
thickness not in uniform size because of many factor such as compressive forces
during manufacturing ,type of tabetting method and etc.
2.Hardness :
Most common range of hardnesss for paracetamol tablet from samples is 89.8 mm
till 119.00 mm.Theoretically in market the hardness range start with 58 mm till
297 mm but it is depend on the dosage given and type of tablet either sustained
release drug or uncoated tablet. As increase the hardness as increase the
disintegration period.
The
standard deviation from the table show limit for tablet to be released to
market must be not more and less than 5 % (5.650 mm).But unfortunately 3
samples(sample 5,6 and 8) from 10 samples more than more and less than ( 5.650
mm ) and another 7 samples still within the ranges.
The
standard deviation more than (5 %) accepted batch influence by many factor
amount of binder,compression of tablet and compressive forces and method of
granulation in preparing the tablet (wet method gives more hardness than direct method give the best hardness)
Uniformity of
Hardness is important cause it can affect the disintegration. If the tablet is
too hard it may not disintegrate in the required period of time.And if the
tablet is too soft it will not withstand the handling during subsequent
precessing such as coating and packaging. By ensure the uniformity the need for
pressure adjustment on tabletting machine.Therotically the normal
total of hardness between 40 till 60 N however certain tablet are intened to
dissolve slowly deliberate higher hardness value.
3.Diameter :
From
the result using 10 sample of tablet ( paracetamol 500 mg ) , average of
diameters are 13.106 mm . it is shows that the tablet approved because not more
and less than 3%
( 0.164mm ) of standard deviation.
( 0.164mm ) of standard deviation.
Tablet
thickness important test for tablet packaging because of that the uniformity of
thickness is needed.Very thick tablet affect in packaging either in blister or
plastic
container.Tablet thickness influence by die of tableting process.
container.Tablet thickness influence by die of tableting process.
Conclusion
:
Without
proper normalisation of tablet hardness and compression force data, misleading
conclusions may be drawn on formulation behaviour particularly when using
different equipment for tableting. We have shown how important the tablet
thickness and punch diameter is to normalise the tablet hardness and
compression force data to give meaningful comparative data.
Experiment 2: Tablet Friability
Introduction
The tablet is a compact of solid
particles designed for drug delivery. It is a preferred
dosage form because it is relatively
economical to produce, has superior stability and dose
accuracy. Tablet design is however a complex process
because it must satisfy several
competing objectives. For example,
tablets must be mechanically strong to sustain stresses
during handling but not too strong to
hinder appropriate drug release. An
optimum mechanical
strength is thus required to maintain
the elegance of a tablet and to perform desired drug delivery
function.
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. It can be caused by a number of factors including poor tablet design
(too sharp edges), low moisture content, insufficient binder, etc.
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. Based on an original
design by Roche, the friability tester has now become an accepted standard
throughout the pharmaceutical industry for determining the resistance of
uncoated tablets to the abrasion and shock experienced in manufacturing,
packing and shipping operations
Objectives
1.
To describe the procedure for
the Friability Testing.
2.
To evaluate
a tablet product in terms of tablet friability, with the weight variation.
Procedures
1.
10 tablets were selected and
weighed.
2.
All tablets were put into the
drum of tablet abration and friability tester. Rotation was set to 100rpm up to
10 minutes and the operation was started.
3.
All the tablets were removed
and freedom from dust or powder was ensured using the brush at the end of the
operation.
4.
The tablets were reweighed and
the percentage loss of weight was determined.
Results and calculation
Tablet used: Ettrocin 250mg Film coated
tablet
As antibiotics against infection
caused by susceptible microorganisms.
Initial weight of 10 tablets: 6.624g
Final weight of 10 tablets: 6.5758g
Differences in weight of 10 tablets:
(6.624-6.5758)g
=0.0482g
Percentage loss of weight: 0.0482/6.624g
x 100%
=0.73%
Discussion
Experiment 3 Uniformity of weight of tablets and capsules.
Introduction
To ensure the consistency of dosage units, each unit in a given batch should contain the active drug within a narrow range around the label claim. The uniformity of dosage units can be evaluated either by measuring the content uniformity or the weight of the tested units The test for weight variation is applicable for hard capsules, uncoated tablets and film-coated tablets containing 25 mg or more of a drug substance comprising 25% or more, by weight, of the dosage unit or, in the case of hard capsules, the capsule contents, except that uniformity of other drug substances present in lesser proportions is demonstrated by meeting the requirements for content uniformity. Unless the 25 mg/25% threshold limit is met, the use of the mass/weight variation test as an alternative test for content uniformity is not considered interchangeable in all International Conference on Harmonization (ICH) regions (The United States Pharmacopeial Convention, 2011; International Conference on Harmonization, 2008). The test for content uniformity is required for all dosage forms not meeting the above conditions for the weight. These tests are necessary to ensure that patients take a precise pharmaceutical dose. This issue is of high importance not only for whole tablets but also for the obtained halves in cases of tablet splitting since the resultant splits are essentially the new dosage form for the patient. In fact, tablet splitting is a known, widely spread, and an accepted practice in the field of pharmacy. The reasons behind this practice include providing the patient with the desired dose if the product is not available in the required strength, starting therapy with the lowest possible doses to reduce the incidence of side effects of certain drugs, reducing medication costs, and making the swallowing of large tablets easier
Introduction
To ensure the consistency of dosage units, each unit in a given batch should contain the active drug within a narrow range around the label claim. The uniformity of dosage units can be evaluated either by measuring the content uniformity or the weight of the tested units The test for weight variation is applicable for hard capsules, uncoated tablets and film-coated tablets containing 25 mg or more of a drug substance comprising 25% or more, by weight, of the dosage unit or, in the case of hard capsules, the capsule contents, except that uniformity of other drug substances present in lesser proportions is demonstrated by meeting the requirements for content uniformity. Unless the 25 mg/25% threshold limit is met, the use of the mass/weight variation test as an alternative test for content uniformity is not considered interchangeable in all International Conference on Harmonization (ICH) regions (The United States Pharmacopeial Convention, 2011; International Conference on Harmonization, 2008). The test for content uniformity is required for all dosage forms not meeting the above conditions for the weight. These tests are necessary to ensure that patients take a precise pharmaceutical dose. This issue is of high importance not only for whole tablets but also for the obtained halves in cases of tablet splitting since the resultant splits are essentially the new dosage form for the patient. In fact, tablet splitting is a known, widely spread, and an accepted practice in the field of pharmacy. The reasons behind this practice include providing the patient with the desired dose if the product is not available in the required strength, starting therapy with the lowest possible doses to reduce the incidence of side effects of certain drugs, reducing medication costs, and making the swallowing of large tablets easier
Tablets
1. The tablets used in this experiment are
non-steroidal anti-inflammatory analgesic (Mefonomic acid B.P.
500mg).
2. 20 tablets are weighed. The average weight was
shown in the calculation part below.
3. Tablets was weighed individually and for each
tablet, the percentage of deviation of its weight from the average weight was calculated and shown in
the result.
4. The deviation of individual weight from the average
weight should not exceed the limits given below.
Average weight of tablet
|
Deviation (%)
|
Number of tablets
|
Less than 80 mg
|
+ 10.0
+ 20.0
|
Minimum 18
Maximum 2
|
80mg to 250 mg
|
+ 7.5
+ 15.0
|
Minimum 18
Maximum 2
|
More than 250 mg
|
+ 5.0
+ 10.0
|
Minimum 18
Maximum 2
|
The percentage of deviation is
calculated using the formula as below.
Net weight of capsules - average net weight of capsules x 100%
average net weight of capsules
1. The capsules used in this experiment are antibiotic
(Amoxycillin Trihydrate B.P. equivalent to Amoxycillin B.P. 250mg).
2. 20 capsules are selected at random.
3. One capsule was weighed. The capsule was opened and
the contents are removed as
completely as possible. The emptied shells are
weighed. The net weight of its contents are
determined, that is by subtracting the weight of
shells from the weight of the intact capsule.
4. The procedure are repeated with another 19
capsules.
5. The average net weight are determined from the sum
of individual net weights.
6. The percentage of deviation from the average net
weight for each capsules are determined.
The deviation of individual net weight should not
exceed the limits given below.
Average net weight of capsule
|
Deviation (%)
|
Number of capsules
|
Less than 300 mg
|
+ 10.0
+ 20.0
|
Minimum 18
Maximum 2
|
300mg and more
|
+ 7.5
+ 15.0
|
Minimum 18
Maximum 2
|
The
percentage of deviation is calculated using the formula as below.
Net weight of capsules - average net weight of capsules x 100%
average net weight of capsules
Results
Tablets
Tablet
|
Weight (mg)
|
Percentage of deviation (%)
|
1
|
588.8
|
+0.65
|
2
|
580.9
|
-0.70
|
3
|
592.1
|
+1.21
|
4
|
585.6
|
+0.10
|
5
|
582.9
|
-0.36
|
6
|
587.0
|
+0.34
|
7
|
587.5
|
+0.43
|
8
|
585.2
|
+0.03
|
9
|
588.9
|
+0.67
|
10
|
580.9
|
-0.70
|
11
|
577.6
|
-1.26
|
12
|
587.9
|
+0.50
|
13
|
582.7
|
-0.39
|
14
|
576.4
|
-1.47
|
15
|
582.8
|
-0.38
|
16
|
580.4
|
-0.79
|
17
|
584.7
|
-0.05
|
18
|
595.3
|
+1.76
|
19
|
584.6
|
-0.07
|
20
|
588.3
|
+0.12
|
Average
|
585.0
|
-
|
Capsules
Capsule
|
Weight (mg)
|
Weight of shell (mg)
|
Net weight
|
Percentage of deviation (%)
|
1
|
359.1
|
64.4
|
294.7
|
-2.29
|
2
|
360.1
|
63.1
|
297.0
|
-1.53
|
3
|
368.3
|
63.1
|
305.2
|
+1.19
|
4
|
355.0
|
63.2
|
291.8
|
-3.25
|
5
|
374.7
|
62.9
|
311.8
|
+3.38
|
6
|
371.6
|
64.7
|
306.9
|
+1.76
|
7
|
373.8
|
63.0
|
310.8
|
+3.05
|
8
|
352.1
|
62.0
|
290.1
|
-3.81
|
9
|
369.6
|
62.6
|
301.0
|
-0.20
|
10
|
359.9
|
64.1
|
295.8
|
-1.92
|
11
|
371.3
|
64.2
|
307.1
|
+1.82
|
12
|
366.5
|
64.2
|
302.3
|
+0.23
|
13
|
369.8
|
61.5
|
308.3
|
+2.22
|
14
|
362.2
|
62.5
|
299.7
|
-0.63
|
15
|
351.1
|
62.3
|
288.8
|
4.24
|
16
|
381.4
|
62.5
|
318.9
|
+5.74
|
17
|
362.3
|
64.6
|
297.7
|
-1.29
|
18
|
362.5
|
63.8
|
298.7
|
-0.96
|
19
|
364.1
|
63.7
|
300.4
|
-0.40
|
20
|
369.1
|
63.9
|
305.2
|
+1.19
|
Average
|
301.6
|
-
|
||
Calculations
1. Average weight of tablet
= Total weight of 20 tablets
20
= 585.025 mg
≈ 585.0mg
2. Average net weight of
capsule
= Total net weight of 20 tablets
20
= 301.615mg
≈ 301.6mg
Discussion
To ensure the consistency of dosage units, the test for
uniformity of weight was carried out. The test for weight variation is
applicable for hard capsules, uncoated tablets and film-coated tablets. According
to the result obtained, the tablets used has an average weight of 585.0mg and
it is in the category of ‘250mg and more’. All the 20 tablets did not exceed
the limit of + 5.0% and therefore consider a successful badge of
tablets. For the capsules, all 20 capsules have average net weight of 301.6mg.
Therefore it is the ‘300mg and above’ category. All the capsules have the percentage
of deviation within the + 7.5%, therefore all of the 20 capsules pass
the test.
Reference
http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3745048/
Experiment 4 Dosage performance tests.
Objectives :
Apparatus and material :
For disintegration test,
500 mL distilled water, 500 mL beaker, disintegration machine (include disc, mechanical device to control up-down movement (28-32 cpm), device to control temperature (37 °C))
For dissolution test,
1000mL cylindrical vessel, motor to regulate paddle speed, water bath (37°C)
Introduction
The performance test is one of a series of tests that
compose the specification in a United States Pharmacopeia (USP) dosage form
monograph. For an orally administered, nonsolution dosage form, it is usually
satisfied by either a dissolution or disintegration procedure. Complete disintegration is defined as that state in which any residue of the unit, ecvept fragments of insoluble coating or capsule shell, remaining on the screen of the test appartus or adhering to the lower surface of the disc, if used, is a soft mass having no firm core. Dissolution
acceptance criteria are usually set in private negotiations between an
applicant and a regulatory agency. With information about this private
agreement and other information provided in a sponsor's Request for Revision to
USP, the USP's Council of Experts elaborates a public dosage form monograph.
Based on the relationship between the regulatory decisions and the Request for
Revision, the USP dissolution procedure links to a regulatory judgment about
bioavailability and bioequivalence and, ultimately, to a judgment about safety
and efficacy. The current dissolution procedure and acceptance criteria are
perceived as having worked well over the years and are generally accepted.
Objectives :
- The objectives for disintegration test is to determine how long the time taken needed to tablet for disintegrate and whether it is disintegrate properly when placed in a liquid medium under the experimental condition in this experiment.
- The objectives for dissolution test is to determines the amount of active ingredient(s) released from a solid oral dosage form, such as a tablet or a capsule, using a known volume of dissolution medium within a predetermined length of time. This test method may not be applicable to certain oral dosage forms.
Apparatus and material :
For disintegration test,
500 mL distilled water, 500 mL beaker, disintegration machine (include disc, mechanical device to control up-down movement (28-32 cpm), device to control temperature (37 °C))
For dissolution test,
1000mL cylindrical vessel, motor to regulate paddle speed, water bath (37°C)
Disintegration
test procedure
1. The disintegration
test equipment was set up by following the instruction in the manual of
operation.
2. 500 mL of distilled
water was added into the beaker and then added to the disintegration machine. Then, the water was left until the
temperature of water is about 37°C .
3. The time was set up to
60 minutes. Three tablet of the same types was added into each tube with
another 3 tablet from another group. Then, the disk was added into each tube
before started the operation.
4. The tablet in each
tube was checked whether it is pass the test or not at the end of the
operation.
5. The tablets pass the
test if all 3 tablets disintegrate within 60 minutes. If there is any tablet
that does not disintegrate, we must pressed the tablet and if the tablet was
disintegrate when we press, it also means that the tablet comply with the test.
Procedures of Dissolution test for tablets
1.
Dissolution vessel was filled with the buffer
solution to 900 ml mark. The temperature was setted to 37°C.
2.
One Ibuprofen Tablet was placed into each dry
basket assembly.
3.
The
stirring speed was setted to 150 rpm. The basket assembly was lowered into
position in the vessel and the operationwas stated.
4.
10 ml samples of the dissolution medium was withdrawed using syringes that include
with filter to prevent any solid d particle from drug enter the solution from
each vessel for analysis and filter the solution 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 10 mm
from the wall of the vessel.
5.
A
standard solution of ibuprofen was prepared by diluting 10.0 mg of ibuprofen
reference standard to 50 ml with dissolution medium.
6.
2.0 ml of sample solution was dilluted and 2.0 ml
of standard solution to 25 ml with dissolution medium in separate 25 mL of
volumetric flasks.
7.
The
absorption of both solutions was measured in a 1 cm cell at a wavelength of 221
nm.
8.
The percentage of amount of ibuprofen dissolved was calculated
using the following formula:
At/As × W×
P × 900 × 25/2 × 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.
9. From the
results obtained, determine whether the tablets comply with the requirements of
the United States Pharmacopoeia. USP limits: Not less than 75% of the stated
amount of C13H18O2 dissolved in 30 minutes.
Result and Calculations
The Uphamol tablet was disintegrate completely at 5.30 minutes.
Percent of ibuprofen dissolve :
Percent of ibuprofen dissolve :
At/As
× W× P × 900 × 25/2 × 100/200
=
0.667/3.436 x 0.02 x 0.98 x 900 × 25/2 × 100/200
=21.40%
Discussion
The error during disintegration test experiment is the water in the beaker may not heat up adequately. So, these may affect the disintegration process. Then, the tablet was expired. So, it may affect the disintegration rate.
For dissolution, 21.40%
< 75 % amount of ibuprofen dissolve thus it doesn’t dissolve and achieve the USP standard .The tablet may seem to be dissolve in the dissolution medium because of the substituent present but the present of active ingredient does not evently distributed throughout the medium thus the percentage of active ingredients is low.This indicate the active ingredient does not soluble quickly and need more time to soluble completely.An error might also occur while conducting the experiment that will affect the percentage.We need to follow this recommended procedure to obtain more accurate percentage,Ensure that the equipment has been calibrated within the past 6-12
months.
Place the volume of dissolution medium, as stipulated in the individual monograph, in the vessel; assemble the apparatus and place it in the water-bath; allow the temperature of the dissolution medium to reach 37±0.5°C and remove the thermometer.When apparatus "Paddle" is used, allow either one tablet or one capsule of the preparation to be tested to sink to the bottom of the vessel before starting the rotation of the blade, taking care that no air bubbles are present on the surface of the dosage form. In order to stop the dosage form from floating, anchor it to the bottom of the vessel using a suitable device such as a wire or glass helix.
When apparatus "Basket" is used, place either one tablet or one capsule of the preparation to be tested in a dry basket at the beginning of each test. Lower the basket into position before rotation.
Immediately start rotation of the blade or basket at the rate specified in the individual monograph for filtration of the removed liquid, use an inert filter with a suitable pore size. Use a filter that does not cause significant adsorption of the active ingredient from the solution, and does not contain substances extractable by the dissolution medium that would interfere with the specified method of analysis. Use centrifugation as an alternative with conditions depending on the sample being tested.
Place the volume of dissolution medium, as stipulated in the individual monograph, in the vessel; assemble the apparatus and place it in the water-bath; allow the temperature of the dissolution medium to reach 37±0.5°C and remove the thermometer.When apparatus "Paddle" is used, allow either one tablet or one capsule of the preparation to be tested to sink to the bottom of the vessel before starting the rotation of the blade, taking care that no air bubbles are present on the surface of the dosage form. In order to stop the dosage form from floating, anchor it to the bottom of the vessel using a suitable device such as a wire or glass helix.
When apparatus "Basket" is used, place either one tablet or one capsule of the preparation to be tested in a dry basket at the beginning of each test. Lower the basket into position before rotation.
Immediately start rotation of the blade or basket at the rate specified in the individual monograph for filtration of the removed liquid, use an inert filter with a suitable pore size. Use a filter that does not cause significant adsorption of the active ingredient from the solution, and does not contain substances extractable by the dissolution medium that would interfere with the specified method of analysis. Use centrifugation as an alternative with conditions depending on the sample being tested.
Reference
http://apps.who.int/phint/en/p/docfr/docfl,doc,d,Jb.1.html
http://www.pharmainfo.net/disintegration-test
http://www.ncbi.nlm.nih.gov/pubmed/15783064
http://www.pharmainfo.net/disintegration-test
http://www.ncbi.nlm.nih.gov/pubmed/15783064
http://apps.who.int/phint/en/p/docf/
Experiment 5 Content of ibuprofen (assay)
Objectives
- To determine the actual content of Ibuprofen in Ibuprofen tablet.
Procedures
- 20 Ibuprofen tablets were weighed and crushed into powder using pestle and mortar.
- A quantity of powder was measured to contain exactly 0.5 g ibuprofen and then the powder was extracted with 20 ml chloroform for 15 minutes.
- The mixture was filtered through a filter paper.
- The residue was washed with 3 times of 10 ml chloroform and the combined filtrate was exposed to hot air to help it evaporate. The residue the was dissolved in 100 ml ethanol 96% that was previously neutralized to phenolphthalein solution.
- The solution was titrated with 0.1 M sodium hydroxide until the end point, in which the solution turned pink. The content of ibuprofen was calculated if each ml 0.1 M NaOH is equivalent to 0.02063 g of ibuprofen.
Result
1
tablet ibuprofen = 0.2 g ibuprofen
20
tablets = 4.0 g ibuprofen
Mass
of 20 tablets ibuprofen = 8.2444 g
8.2444
g = 4.0 g ibuprofen
For 0.5 g ibuprofen ; 8.2444 g / 8 = 1.03055 g
Volume
of NaOH used = 17.7 ml
1 ml
of NaOH = 0.02063 g ibuprofen
17.7
ml NaOH = 0.02063 g x 17.7 = 0.365151 g ibuprofen
Percentage deviation = ( 0.5 - 0.365151 ) x 100 / 0.5 = 26.97 %
Discussion
In this experiment, it is expected that the final mass of ibuprofen calculated from the volume of sodium hydroxide, NaOH is 0.5 g. However, the calculated value is 0.365151 g, which is 26.97 % deviation. If the content of ibuprofen is expected to be 0.5 g, then the volume of NaOH used for titration process should be around 24.2 to 24.3 ml. This deviation occur may be due to errors during the experiment or comes from the tablet itself, that is the tablet may expired already.
1. What are the objectives of the tests for uniformity of diameter and uniformity of content ?
Content uniformity test is used to ensure that every tablet contains the amount of drug substance intended with little variation among tablets within a batch and to determine whether the individual contents are within limits set with reference to the average content of the sample. Tablet diameter is an important quality control test for tablet packaging which affects packaging either in blister or plastic container.Tablet thickness is determine by the diameter of the tablet.
2. State the types of tablets and capsules that must be tested for for uniformity of diameter and uniformity of content.
Type of tablet or capsule that need to undergo test
uniformity of diameter and weight?
1) Uncoated
Tablet
2) Effervescent Tablet
3) Hard capsule
4) Soft Capsule
5) Modified Release Tablet/capsule
6) Enteric-coated tablet/capsule
3. Give reasons for the non-compliance to test for uniformity of weight.
The reason to carry out the test for uniformity of weight for the non-compliance is because of the uneven feeding of granules into the die. Besides, the irregular movement of the lower punch will result in the variation in capacity of die space and have to carry out the test. If we do not mix the ingredients well at blending stage or do not weight the amount of ingredients accurately, this will also produce those non-compliance.
4. Why does dissolution test suitable to be used for batch to batch quality control?
- As an essential part of product development
- In support of an application for a waiver of bioequivalence testing
- To obtain information on test batches used in bioavailability/bioequivalence studies and pivotal clinical studies to support specifications for quality control
- To demonstrate batch-to-batch and lot-to-lot consistency during manufacture, and to indicate potential problems of bioavailability i.e. as a tool in quality control.
5. Explain the difference found in the procedure for dissolution test in the United States Pharmacopoeia and the British pharmacopoeia
In USP, the dissolution procedure consists of three stages, in which the next stage is proceeded only if the previous stage is failed. For Stage 1, 6 tablets of capsules are tested and each unit must not less than (Q + 5)% , Q is percentage dissolved. If not, stage 2 is carried out with another 6 units, and the average of 12 units total is equal to or greater than Q and no unit is less than (Q - 15)%. Then stage 3 is carried out if stage 2 fails. This time the number of tablets or capsules used are 12 units and the average of 24 units total is equal to or greater than Q, not more than 2 units are less than (Q - 15)% and no unit is less than (Q - 25)%.
In BP, the test is carried out with 6 units of tablets or capsules and the result should be, for each unit tested, the amount dissolved is not less than 70% of the active ingredient within 45 minutes. If one unit fails to meet this requirement, a retest of another 6 units are carried out and the requirement is the same for all unit but one of the total units.
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