Experiment 5 Selected Tests on Finished Aspirin and Acetaminophen

Tablets
Uniformity of Dosage, Assay, Dissolution Profile
By Amanda Grennan
Partner Justin Williams
Performed on March 11, 2016 and March 18, 2016
Submitted to Jenny Cortez-Cordova
On April 1, 2016

Objective

To perform selected tests on finished aspirin and acetaminophen tablets. To

perform a Dissolution Profile test on aspirin tablets, which is a chemical test
and a physical test on 6 tablets to determine their strength. To perform an
assay strength test on 10 weighed and finely powdered acetaminophen
tablets to determine the strength of the tablets and how much active
ingredient is present. To perform a Uniformity of Dosage Units test on
acetaminophen, which is a chemical test on 10 tablets to determine the
strength and amount of active ingredient per tablet and compare to the label
claim.

Material and Methods

Refer to Pharmaceutics Laboratory Manual pg 14-20, 104, 76.

Acetaminophen House Method #001 Pharmaceutics Laboratory Manual
Dissolution Profile Testing of Acetaminophen Tablets by UV. Refer to USP
<711> Dissolution. Refer to Uniformity of Dosage Units Weight Variation
Method <905>.
Safety Information
Acetaminophen Slightly hazardous in case of skin contact (irritant), of eye
contact (irritant), of ingestion of inhalation. Tablets: 325mg Equate
(L)1K214PA6 exp Nov 2014. Acetaminophen USP Powder (L)CC003881.
Methanol Clear, colourless, flash point 11C. Poison. Causes eye and skin
irritation. May be absorbed through skin. Flammable liquid and vapour. May
be fatal or cause blindness if swallowed. Causes respiratory tract irritation.
Company: ACP, (L)F1215.
Aspirin/ O-Acetylsalicylic acid 99% White. May cause skin irritation. Causes
respiratory tract irritation. Causes respiratory tract Tablets: 325mg Equate
(L)5111913SKL exp June 2019. Power: Company Aesar exp 05/08 (L)03803.
Ethyl alcohol Clear, colourless flammable liquid. Causes severe eye
irritation. May cause blindness if swallowed. May be fatal if swallowed. May
cause skin irritation. May cause central nervous system depression. May

cause liver and kidney damage. May be absorbed through skin. Company:
ACP, (L)F1215.
Hydrochloric Acid Corrosive liquid. Causes eye and skin burns. May cause
severe respiratory tract irritation with possible burns. May cause severe
digestive tract irritation with possible burns. Company: ACP, (L)H3012.

Results and Interpretation

Active Ingredient: Acetylsalicylic acid/Aspirin

Test Performed: Dissolution Profile House Method #001. USP <711>
Purpose: To test the strength and of 5 tablets in comparison to a standard
solution using a Vanderkamp 600 6-Spindle Dissolution Tester at 50rpm at
time intervals of 10 min, 20 min, and 30. To perform dilutions of the samples
at each specified time and read their absorbencies and the standards
absorbance at 244nm. To calculate the % ASA dissolved at each specified
time.
Deviations: Aspirin was used for this test, not acetaminophen. One spindle
was not working on the Dissolution Tester, so only 5 tablets were tested, not
6.
Results:
10 minute analysis
Samples: 0.0372; 0.0376, 0.0330, 0.0305, 0.0335
Standard: 0.0940
20 minute analysis
Samples: 0.0756, 0.0898, 0.0861, 0.0891, 0.0803
Standard: 0.1002
30 minute analysis
Samples: 0.0780, 0.0726, 0.0776, 0.0758, 0.0881, 0.0821
Absorption of Standard: 0.0730
Calculations:
10 minutes:
Average absorption of samples =
(0.0372+0.0376+0.0330+0.0305+0.0335) / 5 = 0.03436

% acetaminophen dissolved =

0.03436
0.0940

0.0067 mg/ml
0.007 mglml

x 100 = 34.99%

20 minutes:
Average absorption of samples = (0.0756+0.0898+0.0861+0.0891+0.0803)/
5 = 0.08418
0.08418
0.0067 mg/ml
% acetaminophen dissolved =
x
x 100 +
0.1002
0.007 mglml
(5 x 34.99)
= 80.61%
900
30 minutes
Average absorption of samples =
(0.0780+0.0726+0.0776+0.0758+0.0881+0.0821)/ 6 = 0.0790
0.0790
0.0067 mg/ ml
% acetaminophen dissolved =
x
x 100 +
0.0730
0.007 mglml
5 x (34.99+80.61)
= 104.22%
900
Interpretation: The dissolution profile testing of aspirin tablets by UV passed
for strength as there was an increase in aspirin dissolved over time.
Questions:
1.

Dissolution Profile of Aspirin

2. Yes, the percent dissolved at 30 minutes for the single point dissolution
test would be similar to the result obtained from the dissolution profile
at 30 minutes.
3. Both 30 minute points would be similar because they are both testing
the percentage of release at that specified time of the same active
ingredient. The only difference between the two tests is that the
dissolution profile gives enough points to produce a dissolution curve,
whereas the dissolution test only provides us with one data point.

Active Ingredient: Acetaminophen

Test Performed: Assay
Purpose: To perform an assay test on 10 weighed and finely powdered
acetaminophen tablets to test for the strength and determine how much
active ingredient is present in each tablet and relate to the bottle claim. The
acceptance criteria is 90.0 110.0%.
Deviations: Modified procedure refer to Pharmaceutics Lab Manual p. 15.
Results:
Mass of 10 tablets: 3617.3mg
Mass of crushed tablets added: 113.3mg (added to 100mL volumetric flask)

Mass used for standard: 111.3mg

Area standard: 459.7520
Area sample (average): (423.2160+428.5630)/2 =
Refer to attached print-outs.

425.8895

Calculations:
Target Weight x

Avg Tabl e t Weight

Label Claim

= 100mg x

3617.3 m g /10
325 m g

Theoretical weight of acetaminophen in sample = 113.3g x

101.80mg
Theoretical sample concentration =
Standard conc =
425.8895
459.7520

111.3 mg
100 mL

0.1113mg/mL
0.1018 mg/ml

101.80 mg
100 mL

= 111.30mg
325 m g
3617.3 mg/10

x (10/100) = 0.1018mg/mL

x (10/100) = 0.1113mg/mL
x 100% = 101.28% acetaminophen/tablet

Interpretation: The assay test does not produce a pass or fail result, however
101.28% acetaminophen per tablet is not possible, so experimental error
occurred within the experiment. Possible sources include contamination or
random instrumentation error.
Questions:
1. In the modified assay procedure, Portion of the powder equivalent to
means to weigh the sample powder in an amount equal to the USP
powder.
Avg Tablet Weight
2. We used the equation Target Weight x
to determine
Label Claim
how of the sample should be added to the 100mL volumetric flask for
examination.
3. For Uniformity of Dosage testing by Weight Variation, we use the assay
result in order to calculate the content of active ingredient in each of
the 10 tablets individually.

Test Performed: Uniformity of Dosage Units Weight Variation Method

<905>.
Results: Weights of 10 tablets: 0.3654g, 0.3556g, 0.3560g, 0.3596, 0.3708g,
0.3669g, 0.3548g, 0.3599g, 0.3627g, 0.3638g
Calculations:

Average tablet weight =

(0.3654g+0.3556g+0.3560g+0.3596+0.3708g+0.3669g+0.3548g,
0.3599g+0.3627g+0.3638g) / 10 = 0.3616g
0.3654 g
0.3616

x 101.28% = 102.34%

0.3556 g
0.3616

x 101.28% = 99.60%

0.3560 g
0.3616

x 101.28% = 99.71%

0.3596 g
0.3616

x 101.28% = 100.72%

0.3708 g
0.3616

x 101.28% = 103.86%

0.3669 g
0.3616

x 101.28% = 102.76

0.3548 g
0.3616

x 101.28% = 99.38%

0.3599 g
0.3616

x 101.28% = 100.80%

0.3627 g
0.3616

x 101.28% = 101.59%

0.3638 g
0.3616

x 101.28% = 101.90%

Using Microsoft Excel:

- Standard Deviation: 1.49%
- Mean: 101.27%
RSD = 100(1.49) / 101.27 = 1.47%
Interpretation: The acetaminophen tablets passed for strength as the results
lie within the range of 85.0% 115.0% of the label claim and the RSD is less
than 6.0%.

Summary Table

Test
Dissolution
Profile

Assay

Uniformity of
Dosage Units

USP
Specifications/
Conditions
The dissolution
of aspirin
increased as a
function of time
to produce a
dissolution
curve.
Calculate the %
acetaminophen
per tablet.
All values lie
within the
acceptance
criteria of 85.0%
and 115.0% and
the RSD is equal
or less than
6.0%.

Result

Pass/Fail

A dissolution
curve was
constructed. The
amount of
aspirin dissolved
increased as
time increased.
101.28% of
acetaminophen
per tablet was
calculated
The mean was
101.27% and all
values lie within
the acceptance
criteria. The RSD
was 1.47%.

Pass

Pass

Pass

Conclusion
Finished product tests were performed on Aspirin tablets and Acetaminophen
tablets to determine their strength. The aspirin tablets tested positive in the
Dissolution Profile test because the amount of aspirin dissolved increase over
time. The acetaminophen tablets tested positive in the Uniformity of Dosage
Units test because the result was within USP specifications. After performing
the Assay test, the tablets were calculated to contain 101.28%
acetaminophen per tablet. According to these results, the aspirin and
acetaminophen tablets meet the requirements for use, sale, and distribution.

References

Pharmaceutics Laboratory Manual pg 14-20, 104, 76. Acetaminophen House

Method #001 Pharmaceutics Laboratory Manual Dissolution Profile Testing
of Acetaminophen Tablets by UV. Refer to USP <711> Dissolution. Refer to
Uniformity of Dosage Units Weight Variation Method <905>.