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UV-Vis Estimation of Paracetamol & Ibuprofen

The document outlines an experiment aimed at the simultaneous estimation of paracetamol and ibuprofen using a UV spectrophotometer. It details the objectives, principles, methods, and procedures for preparing solutions and analyzing a tablet formulation. The results indicate the percentage purity of paracetamol and ibuprofen in the Combi flam tablet as 85.08% and 108% respectively.

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Sanket Narigara
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0% found this document useful (0 votes)
497 views4 pages

UV-Vis Estimation of Paracetamol & Ibuprofen

The document outlines an experiment aimed at the simultaneous estimation of paracetamol and ibuprofen using a UV spectrophotometer. It details the objectives, principles, methods, and procedures for preparing solutions and analyzing a tablet formulation. The results indicate the percentage purity of paracetamol and ibuprofen in the Combi flam tablet as 85.08% and 108% respectively.

Uploaded by

Sanket Narigara
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as DOCX, PDF, TXT or read online on Scribd

EXPERIMENT NO: 02

AIM: SIMULTANEOUS ESTIMATION OF PARACETAMOL AND IBUPROFEN


USING UVSPECTROPHOTOMETER

OBJECTIVES:
1) Understand theory of simultaneous estimation of drugs by UV.
2) Determine percentage of paracetamol and ibuprofen by simultaneous estimation method using UV
spectrophotometer.
METHOD: Simultaneous equation method.

PRINCIPLE:
Simultaneous Equation Method (Vierodt’s Method) is one of the most common and easier methods
employed for Spectrophotometric multi-component analysis in the concentration of several components
present in the given mixture can be determined in solving a set of simultaneous equations even if their
spectra overlap. This method derives the principle from the additive nature of absorbance of individual
components in any mixture. Suppose a sample contains two absorbing species X and Y. Absorbance of this
mixture is measured at wavelengths of maximum absorbance (λmax) of each drug λ1 for drug y and λ2 for
drug x. Thus, the individual concentrations of both drugs may be determined using a simultaneous equation
method provided that certain criteria are fulfilled.

THEORY:

Drugs whose amounts are to be estimated are-


1. Paracetamol [IUPAC name- N-(4-hydroxyphenyl) acetamide]:

2. Ibuprofen [IUPAC name –(RS)-2-(4-(2-methylpropyl) phenyl) propanoic acid]:

If a sample contains two absorbing drugs (paracetamol and Ibuprofen), both are absorbed at λmax of
each other, so it is possible to determine the concentration of paracetamol and ibuprofen by the technique of
simultaneous equations. The necessary information is required for this purpose. The absorptivity of
paracetamol at λ1 (243nm) and λ2 (223nm) are 𝑎x1 and 𝑎x2respectively.
 The absorptivity of ibuprofen at λ1 (243nm) and λ2 (223) are 𝑎y1 and 𝑎y2respectively.
 The absorbance of the sample at λ1 (243nm) and λ2 (223) are A1 and A2 respectively.
 𝐶x 𝑎𝑛𝑑𝐶y are the concentrations of paracetamol and ibuprofen respectively in the diluted sample.
 Using the below equation concentrations of paracetamol and ibuprofen are calculated.

REQUIREMENTS:
 Glassware’s: Volumetric flask, measuring cylinder, pipette, beaker, glass rod, funnel, weighing
balance, test tubes, test tube stand, mortar, pastel, spatula, etc.
 Chemicals: Paracetamol, Ibuprofen, Methanol, Distilled water, and tablet Combiflam (labeled
claim- Paracetamol- 325mg, Ibuprofen- 400mg)
 Required solvent: 1:1 solution of Methanol and Distilled Water.

PROCEDURE:
1) Preparation of standard stock solution of Paracetamol and Ibuprofen:

Stock 1: Accurately weigh 100 mg of paracetamol and transfer in a 100 ml volumetric flask. Add
Methanol: water solution in a volumetric flask, mix, and make volume to 100 ml. (1mg/ml or 1000µg/ml).

Stock 2: Take 10 ml of sample from stock 1 and transfer it into a 100 ml volumetric flask. Make up the
volume of 100 ml with the methanol-water system. (100µg/ml).
Repeat the same procedure for ibuprofen.
2) Preparation of aliquots:

Prepare six working standard solutions of Paracetamol and Ibuprofen with concentrations of
10,20,30,40,50,60µg/ml in a methanol-water system from stock II solution separately.
3) Determination of λ maximum and calculation of absorptivity:
a) Scan working standard solution of 20 µg/ml (Paracetamol and Ibuprofen) in the entire UV range of
400-200nm for maximum absorbance 243nmλ1 of Paracetamol and 223nm λ2 of Ibuprofen.
b) Measure the absorbance of resulting solutions 1, 2, 3, 4, and 5 µg/ml at both maximum in fixed
wavelength measurement and calculate absorptivity. (Table 3.1 for Ibuprofen and Table 3.2 for
Paracetamol)
4) Analysis of the tablet formulation:
1. Weigh accurately twenty tablets of the marketed formulation.
2. Calculate the average weight and powder it.
3. Transfer a quantity of powder equivalent to 100 mg of paracetamol to a 100 ml volumetric flask and
dissolve in a 100 ml of solvent system. (1mg/ml).
4. Withdraw 10 mL form the above solution and dilute to produce 100 mL (100µg/ml).
5. Filter the sample solution through Whatman filter paper No 41.
6. Withdraw 1 mL filtrate and dilute up to 10 ml (10 µg/ml).
7. Note the absorbance of this solution at both λ maximum.
8. Repeat the same procedure for the Ibuprofen.

Conc. Absorbance
(µg/ml) (223nm)
0 0
1 0.074
2 0.165
3 0.186
4 0.27
5 0.364

Conc. (µg/ml) Absorbance


(243nm)
0 0
1 0.151
2 0.27
3 0.455
4 0.539
5 0.677

RESULT:
The percentage purity of Paracetamol and Ibuprofen in Combi flam tablet was found to be 85.08% w/w and
108% w/w respectively.
CONCLUSION:
The given sample contains 108% Paracetamol and 85.08% of Ibuprofen (amount of drug) in the marketed
Combi flam tablet.

Common questions

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The principle behind the simultaneous estimation of Paracetamol and Ibuprofen using a UV spectrophotometer is based on the Simultaneous Equation Method, also known as Vierodt’s Method. This method involves solving a set of simultaneous equations to determine the concentration of multiple components in a mixture, even if their spectra overlap. The technique relies on the additive nature of absorbance: the total absorbance of a mixture is the sum of the absorbances of its individual components. By measuring the absorbance at the maximum wavelengths (λmax) for each drug—243 nm for Paracetamol and 223 nm for Ibuprofen—one can use known absorptivities (ax1, ax2 for Paracetamol and ay1, ay2 for Ibuprofen) at these wavelengths to form equations involving concentration (Cx and Cy for Paracetamol and Ibuprofen, respectively) and solve them simultaneously .

Filtering the sample solution through Whatman filter paper No 41 during the analysis is a necessary step to remove any undissolved particles or insoluble excipients present in the tablet formulation. This ensures that the resulting solution used for spectrophotometric analysis is clear and free from particulate matter, which could otherwise cause scattering of light and potentially affect the accuracy of absorbance readings and, consequently, the estimation of drug concentrations .

Determining the maximum wavelength (λmax) in UV spectrophotometry is crucial as it ensures the most sensitive and specific detection of the drug components being analyzed. The λmax corresponds to the wavelength where a substance exhibits its highest absorbance, providing optimal conditions to distinguish and measure the components separately despite their overlapping spectra. For Paracetamol, the λmax is 243 nm, while for Ibuprofen, it is 223 nm. Measuring at these specific wavelengths allows the formulation of simultaneous equations based on the drugs' known absorptivity values (ax1, ax2 for Paracetamol; ay1, ay2 for Ibuprofen) to accurately calculate their concentrations in the mixture .

Using a methanol-water solvent system in the spectrophotometry method provides several advantages. It ensures effective solubilization of both Paracetamol and Ibuprofen, maximizing their absorbance readings, which is critical for accurate analysis. Methanol, being polar, promotes dissolution and stabilizes the UV-active species by preventing aggregation, which could impact spectroscopy readings. This solvent system also harmonizes the optical path of light through the sample, ensuring consistent refractive index and minimizing variable light scattering effects, thus enhancing precision in the simultaneous equation method for component concentration estimation .

The experimental results indicate that the percentage purity of Paracetamol in the Combiflam tablet was found to be 85.08% w/w, while Ibuprofen was 108% w/w. These findings suggest that the amount of Paracetamol is below the labeled claim, while Ibuprofen exceeds it. These discrepancies in the drug content can have significant implications: for Paracetamol, reduced content may lead to suboptimal therapeutic effects, whereas for Ibuprofen, exceeding the expected content may increase the risk of side effects. Such variations in drug purity and dosage strength must be addressed to ensure compliance with quality standards and patient safety .

Preparing aliquots with varying concentrations (10, 20, 30, 40, 50, 60 µg/ml) in the spectrophotometry method is significant for establishing a calibration curve, which is essential for determining the linearity and accuracy of the analytical method. These varying concentrations allow the recording of absorbance at multiple points, which can be plotted to produce a standard curve. By demonstrating that absorbance correlates linearly with concentration, the method validates that it can accurately estimate unknown concentrations in sample solutions based on their measured absorbance .

The absorptivity values of Paracetamol (ax1 at 243 nm and ax2 at 223 nm) and Ibuprofen (ay1 at 243 nm and ay2 at 223 nm) at their respective λmax are crucial for forming simultaneous equations to estimate drug concentrations. When absorbance values A1 and A2 are measured at these wavelengths, they provide the basis to create two equations: A1 = ax1*Cx + ay1*Cy and A2 = ax2*Cx + ay2*Cy, where Cx and Cy represent concentrations of Paracetamol and Ibuprofen. Solving this system of equations using the known absorptivity values allows determination of the concentrations of each drug present in the mixture .

The main equipment required for simultaneous estimation of drugs by UV spectrophotometry includes a UV spectrophotometer, volumetric flasks, measuring cylinders, pipettes, beakers, glass rods, funnels, weighing balances, test tubes, test tube stands, mortars, pestles, and spatulas. The essential chemicals include Paracetamol, Ibuprofen, methanol, distilled water, and the tablet formulation such as Combiflam, which has labeled claims of Paracetamol (325 mg) and Ibuprofen (400 mg). Additionally, a solvent system comprising a 1:1 mixture of methanol and distilled water is essential for preparing the solutions .

Several factors could lead to observed variations in estimated drug content versus the labeled claim in the Combiflam tablet. Manufacturing inconsistencies such as improper mixing or compounding errors can result in non-uniform distribution of active pharmaceutical ingredients within the tablet batch. Analytical errors during sample preparation and measurement, such as inaccuracies in weighing or dilution procedures, could also affect results. Degradation of the drug components over time due to exposure to adverse storage conditions might result in reduced potency. Each of these factors could have contributed to the finding where Paracetamol was underrepresented at 85.08% w/w, and Ibuprofen was found to be 108% w/w .

To prepare a standard stock solution for the simultaneous estimation experiment, weigh accurately 100 mg of Paracetamol and transfer it to a 100 ml volumetric flask. Add a methanol-water solution and mix thoroughly, making up the volume to 100 ml to achieve a 1 mg/ml (1000 µg/ml) concentration. Similarly, for Ibuprofen, follow the same procedure. From each stock solution, take 10 ml and transfer it into separate 100 ml volumetric flasks, diluting with the methanol-water system to reach a concentration of 100 µg/ml. This diluted solution acts as Stock II for further analysis .

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