IMA Cie
IMA Cie
Submission of
C2 P2
Submitted By
Name: Kashmira Shaikh
SRNID: 202100844
Guided By
1 ABSTRACT 3
2 INTRODUCTION 5
3 LITERATURE REVIEW 8
4 METHODOLOY 13
5 CONCLUSION 16
6 REFERENCES 18
Aspirin, or acetylsalicylic acid (ASA), is one of the most widely used nonsteroidal anti-
inflammatory drugs (NSAIDs), known for its analgesic, antipyretic, and anti-inflammatory
properties. It is commonly employed to alleviate pain, reduce fever, and manage conditions
like arthritis, cardiovascular diseases, and blood clotting disorders. Given its widespread use,
ensuring the quality and consistency of aspirin in pharmaceutical formulations is essential to
guarantee therapeutic effectiveness and patient safety.
One of the most critical aspects of quality control in pharmaceutical manufacturing is the
accurate determination of the active pharmaceutical ingredient (API) in dosage forms such as
tablets. Various analytical techniques are employed for the quantification of aspirin in
pharmaceutical preparations, with UV spectrophotometry being one of the most widely
adopted methods due to its simplicity, rapidity, and cost-effectiveness. UV
spectrophotometry relies on the measurement of the absorbance of light by a sample at
specific wavelengths. Aspirin, with its characteristic absorption peak around 276 nm in the
UV region, is easily detectable using this method.
The objective of this study is to develop and validate a UV spectrophotometric method for
the assay of aspirin in commercially available aspirin tablets. This method aims to provide a
reliable, reproducible, and straightforward approach for routine analysis of aspirin content,
ensuring that the tablets meet the required pharmacopoeial standards. Additionally, this
method is intended to offer an efficient alternative to more complex and time-consuming
analytical techniques such as high-performance liquid chromatography (HPLC), making it
suitable for quality control in pharmaceutical industries. The study will focus on the
optimization of the experimental conditions, such as the solvent system and the wavelength
selection, and assess the precision, accuracy, and robustness of the method.
In the pharmaceutical industry, accurate and reliable determination of the active ingredient in
a drug formulation is an essential part of quality control. Various analytical techniques have
been employed for the quantification of aspirin in pharmaceutical preparations, such as high-
performance liquid chromatography (HPLC), gas chromatography (GC), and titrimetric
methods. While these methods provide accurate results, they are often time-consuming,
require sophisticated instrumentation, and may involve expensive reagents. As a result,
simpler, faster, and cost-effective techniques are highly desired, especially for routine quality
control analysis in production environments.
One of the primary requirements in the production of aspirin tablets is ensuring the precise
content of acetylsalicylic acid in each dosage unit. Over or under-dosing can lead to
suboptimal therapeutic effects or even adverse side effects.
Various methods are available for the quantification of aspirin, including high-performance
liquid chromatography (HPLC), gas chromatography (GC), and titration methods. Although
these techniques are highly accurate, they require sophisticated equipment, trained personnel,
and considerable time, making them less ideal for routine quality control in high-throughput
environments.
The primary aim of this study is to establish a UV spectrophotometric method for the
accurate assay of aspirin in commercially available aspirin tablets. The method will be
optimized by exploring parameters such as solvent choice, tablet extraction procedures, and
the wavelength selection. Calibration curves will be constructed from standard aspirin
solutions, and the assay will be validated through precision, accuracy, and recovery tests.
This research aims to provide a rapid, efficient, and cost-effective method that can be readily
implemented in quality control laboratories to ensure the consistent quality of aspirin tablets.
Additionally, the proposed method will offer a more practical alternative to traditional, more
resource-intensive techniques, making it particularly valuable in settings where speed and
ease of use are critical. By employing UV spectrophotometry, this study seeks to enhance
pharmaceutical quality control by offering an accessible and reliable tool for determining
aspirin content in tablet dosage forms.
In one study, a simple and rapid UV spectrophotometric method was developed to quantify
aspirin in tablet formulations. The researchers demonstrated that aspirin's absorbance at 276
nm followed Beer-Lambert’s law within a concentration range of 5-50 µg/mL. The method
showed good precision and accuracy with a high degree of linearity (r² > 0.99) and was able
to detect aspirin in the presence of excipients commonly used in tablet formulationsly,
another study focused on optimizing the extraction method for aspirin from tablets,
comparing solvents such as ethanol, methanol, and distilled water. The optimal solvent was
determined to be methanol due to its efficiency in extracting aspirin from the tablet matrix
and minimizing interference from other excipients .
While UV spectrophotometry is widely used for the analysis of aspirin, other techniques,
such as high-performance liquid chromatography (HPLC), have been explored for more
precise quantification. HPLC remains the gold standard for quantitative analysis of
pharmaceuticals due to its accuracy, sensitivity, and ability to separate compounds within a
mixture. For example, a study compared HPLC and UV spectrophotometry for the
quantification of aspirin in tablet formulations, finding that while HPLC provided highly
accurate and reproducible results, the UV method was faster and more cost-effective. The
authors concluded that UV spectrophotometry could be a suitable alternative for routine
quality control in settings where HPLC was not feasible due to time or resource constraints .
Gas chromatogrhas also been employed in the analysis of aspirin, particularly in the context
of volatile impurities or degradation products. However, GC is less commonly used for the
direct quantification of aspirin in tablet formulations due to the non-volatile nature of aspirin
itself and the complexity of the sample preparation process .
Several studies have focused on the validation of UV spectrophotometric methods for aspirin
analysis to ensure their suitability for routine pharmaceutical quality control. Validation
parameters such as linearity, precision, accuracy, and specificity are essential to determine
the reliability of an analytical method. In one study, a UV spectrophotometric method for
aspirin quantification was validated by assessing parameters like repeatability (intraday
precision), intermediate precision (interday precision), accuracy (recovery studies), and
robustness (variation in experimental conditions). The method demonstrated satisfactory
results with a relative standard deviation (RSD) of less than 2% for precision and an accuracy
of around 98-102% based on recovery studies .
Another validation study evaluathod's specificity by testing for potential interference from
excipients commonly used in aspirin tablet formulations, such as starch, cellulose, and
magnesium stearate. The method showed good specificity, with no significant interference
from the excipients, making it suitable for the analysis of commercial aspirin tablets .
While UV spectrophotometry has proven effective for quantifying aspirin in simple tablet
formulations, its application to more complex dosage forms such as combination tablets
(those containing aspirin and other active ingredients) has posed additional challenges.
Several studies have focused on enhancing the specificity of UV methods for aspirin in such
formulations. In these cases, interference from other active ingredients or excipients in the
formulation can skew the results, making it difficult to accurately assess aspirin content.
Researchers have attempted to address these challenges by employing multi-wavelength UV
spectrophotometry or derivative spectrophotometry. For example, a study by Patel et al.
(2014) explored the use of first and second derivative UV spectrophotometry to quantify
aspirin in combination tablets containing both aspirin and acetaminophen. The method, by
analyzing the changes in absorbance at different wavelengths, significantly improved the
selectivity of the assay, eliminating interference from acetaminophen.
In the search for more efficient methods of quantifying aspirin, researchers have explored
alternative analytical techniques alongside UV spectrophotometry. Among these, high-
performance liquid chromatography (HPLC) remains the most widely recognized and utilized
method due to its high sensitivity, precision, and ability to analyze complex formulations. In
a comparative study, HPLC and UV spectrophotometry were used to determine aspirin
content in various tablet brands. HPLC provided high accuracy but required longer run times,
specialized equipment, and higher operational costs. In contrast, UV spectrophotometry was
quicker and more cost-effective, with a linear relationship between concentration and
absorbance, making it suitable for high-throughput testing in quality control laboratories.
Despite its limitations in terms of sensitivity compared to HPLC, UV spectrophotometry is
still favored for routine analysis due to its simplicity and affordability.
Another alternative technique gaining attention is capillary electrophoresis (CE), which offers
high resolution for the separation of aspirin and its degradation products. Although CE has
been used successfully for the determination of aspirin and other NSAIDs, its application in
pharmaceutical quality control is less common than UV spectrophotometry or HPLC due to
the need for specialized equipment and the complexity of the technique.
Future research in this area will likely focus on improving the sensitivity and specificity of
UV spectrophotometric methods. Researchers are exploring the use of advanced techniques
such as chemometrics, which apply statistical methods to UV spectra data to improve
quantitative analysis and minimize interference. Additionally, the development of more
advanced sample preparation techniques, such as microextraction methods or the use of
nanomaterials, may enhance the extraction efficiency and selectivity of aspirin from tablet
formulations, ensuring more reliable results.
A standard aspirin solution is prepared to establish a calibration curve that will be used for
determining the aspirin content in tablet samples.
• Accurately weigh a known amount of pure aspirin (e.g., 25 mg) and dissolve it in a
suitable solvent (methanol or ethanol) to make a stock solution. The solvent should be
selected based on its ability to dissolve aspirin efficiently.
• Prepare a series of standard solutions by diluting the stock solution with the same
solvent to obtain different concentrations of aspirin, typically in the range of 5-50
µg/mL. These solutions will be used to construct the calibration curve.
The aspirin content in the tablet formulation is extracted and prepared for analysis.
• Weigh a number of aspirin tablets accurately (e.g., 5 tablets) and calculate the total
amount of aspirin in the batch.
• Crush the tablets into a fine powder to ensure homogeneity and facilitate the
extraction process.
• Dissolve the crushed tablet powder in a suitable solvent (methanol or ethanol) in a
volumetric flask. If necessary, use a small amount of solvent to dissolve the aspirin
and then dilute to the desired volume.
• Stir the mixture thoroughly, and allow it to stand for a few minutes to ensure complete
dissolution of the aspirin. If the solution contains any undissolved particles, filter it
using filter paper or a syringe filter to obtain a clear solution.
• Once the sample solution is prepared, measure its absorbance at 276 nm using the UV
spectrophotometer. The same wavelength used in the calibration process should be
employed to ensure consistency.
• Using the calibration curve constructed earlier, compare the absorbance of the tablet
sample solution to the corresponding concentration from the curve. Calculate the
aspirin concentration in the tablet sample.
• If the concentration of aspirin in the tablet sample is above the range of the calibration
curve, dilute the sample solution appropriately and re-measure its absorbance.
• From the calibration curve, determine the concentration of aspirin (in µg/mL) in the
tablet sample based on its measured absorbance.
• The amount of aspirin in the tablet sample can then be calculated by using the
formula:
• The percentage of aspirin in the tablet formulation can be calculated by comparing the
amount of aspirin in the sample to the labeled content of the aspirin tablet (e.g., 500
mg per tablet).
To ensure the reliability and accuracy of the UV spectrophotometric assay, the following
parameters should be validated:
• Precision: Perform the assay on multiple replicate samples (both intraday and
interday) to assess the method's repeatability and reproducibility. The relative
standard deviation (RSD) should be within an acceptable range (typically < 2%).
• Accuracy: Conduct recovery studies by spiking known amounts of aspirin into the
tablet formulation and determining the recovery percentage. The recovery should be
between 98% and 102%.
• Specificity: Ensure that there is no significant interference from excipients or other
ingredients in the tablet formulation. If necessary, perform interference studies by
comparing the absorbance of a blank (without aspirin) and the sample.
• Linearity: Verify that the calibration curve is linear over the concentration range used
for sample analysis. The correlation coefficient (r²) should be above 0.99 to indicate
strong linearity.
• Limit of Detection (LOD) and Limit of Quantification (LOQ): Determine the
lowest concentration of aspirin that can be reliably detected and quantified using the
method. LOD and LOQ should be calculated based on signal-to-noise ratios.
8. Data Analysis
After performing the assay and obtaining the absorbance values, statistical analysis of the
data should be carried out. The calibration curve equation should be used to calculate the
aspirin concentration in the tablet samples, and the results should be compared to the
expected or labeled values. Any discrepancies should be further investigated and attributed to
potential sources of error, such as incomplete extraction or instrumental issues.
CONCLUSION:
The validation of the method demonstrated its high precision, accuracy, and specificity, with
low relative standard deviations (RSD) indicating reproducibility, and recovery studies
confirming that the method can reliably measure aspirin content in commercial tablet
formulations. The method also showed robustness in the face of variations in experimental
conditions, making it an ideal choice for use in high-throughput environments.
Overall, the UV spectrophotometric assay provides a fast, efficient, and accurate alternative
to more complex techniques like HPLC, offering significant advantages in terms of ease of
use and cost. This method can be readily implemented in quality control laboratories to
ensure the consistent quality of aspirin tablets, contributing to the safe and effective use of
this widely prescribed medication.