Aim Counterfeit pharmaceuticals are a big concern regarding the issue of medicines due to fake versions containing either the wrong ingredients or inaccuracy of the active ingredient which can cause toxicity issues in patients using these products. The aim of this experiment is to find if the percentage composition of the label (50% paracetamol, 40% aspirin and 10% sucrose) matches that of the percentage composition of the powder by following 10% ranges of each component in the powder. I am going to do this via a number of methods including vacuum filtration, heating, extraction and evaporation.
Experimental method: The experiment was done in three parts: firstly the separation of sucrose, then the separation of Aspirin and the isolation of the unknown component. 1. Separation of Sucrose Weight out and 3. 00g of counterfeit pharmaceutical. Record the weight and transfer the sucrose to 100ml dry conical flask. Add 50ml of dichloromethane to the conical flask containing sucrose. Sucrose is usually liquid so adding organic solvent such as DCM will make the sucrose insoluble making it easy to collect the solid sucrose by vacuum filtration.
Stir the mixture thoroughly containing the sucrose and DCM making sure the solid is dissolved. Filter the solid by vacuum filtration, saving the liquid for the next step into preweghed sample bag and filter paper. Weigh the sample bag containing the sucrose and record the mass of solid sucrose obtained by subtracting form the weight of sample bag and filter paper. 2. Separation of Aspirin Transfer the filtrate form the separation of sucrose to 100ml separating funnel and extract it with two 30ml portions of 5% sodium bicarbonate solution to form sodium acetyl salycilate which is insoluble in DCM.
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For both extractions, use a stirring rod to stir liquid layers until fizzing stops, and place a stopper and shake separating funnel. Transfer the two separate layer solutions to two different 100ml beakers labelling two solutions DCM and aqueous. Return DCM layer to the separating funnel before the second extraction. Combine the two aqueous extracts in one beaker. While stirring with glass rod add slowly 7. 0ml of 6M hydrochloric acid to aqueous extract . test pH of solution with pH strip test and bring the Ph down to 2 or less by adding more acid as required.
Cool solution in ice bath for 10 minutes. Recover solid by vacuum filtration and place in preweighed, labelled sample bag and record the mass. 3. Isolation of unknown component Put solution containing DCM solution form previous step onto gently heated steam bath in a fume cupboard (trying not to boil).
After a while the DCM will start to evaporate and a white solid will be left. Once all DCM evaporates transfer white solid to reweighed sample bag and label.
Results: Mass of Sucrose recovered: 1. 84g Mass of Aspirin recovered: 2.61g Mass of unknown component recovered: 3. 77g Calculations: Percentage recovery: (1. 84g+2. 41g+3. 77g) / 3. 00g = 2. 74% Percentage composition: Sucrose: (1. 84/8. 22)*100 = 22. 0% Aspirin: (2. 61/8. 22)*100 = 32. 0% Unknown: (3. 77/8. 22)*100 = 46. 0% Questions 1. Is the percentage composition on the original container correct? Based on my results and the percentage compositions recovered from the experiment the percentage composition of the powder does not match the percentage composition of the label.
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As the labelled had claimed that the counterfeit pharmaceutical contained (10% Sucrose, 40% Aspirin and 50% of the unknown) which was said to be paracetamol. However the analysis of the counterfeit pharmaceutical produced about 20% sucrose, 30% aspirin and 50% of paracetamol. Also the labelled claimed that the unknown component was paracetamol , although analysis of the unknown sample identified it as Phenactin 2. Describe any evidence that a chemical reaction occurred when you added the 6M HCL to the solution of sodium acetylsalicylate.
A solution of 6M of HCL was added to sodium acetylsalicylate, and the pH of the resultant solution was tested until the pH had gone down to about 2 or less, using the pH paper indicator. 2b. Explain why the changes you observed took place? This change was observed because the HCL was able to convert the salt in acetylsalicylate into the precipitate that was filtered in the separation of aspirin. 3. Describe and explain the effect on you result for the possible experimental errors. Specify which components percentages would be too high or too low and explain why. a.
After adding DCM to counterfeit pharmaceutical at the beginning you didn’t stir the mixture before filtering? The sucrose obtained would not be pure and have lower percentage composition as it would contain impurities of the other components this is because sucrose is insoluble and does not dissolve in DCM, whereas the other components of the mixture are soluble in DCM. So you need to stir the mixture before filtering to make sure all the other components except sucrose are dissolved in DCM. Therefore the only solid that remains undissolved will be the sucrose which can be collected by vacuum filtration.
During the sodium bicarbonate solution extraction, you failed to mix the organic and aqueous solutions thoroughly. The aqueous and organic layers should be fully mixed because aspirin is soluble in DCM and so that sodium acetylsalicylate can move from the insoluble ( DCM layer) to the aqueous soluble layer. c. You mistakenly extracted DCM with 5% HCL than 5% sodium bicarbonate solution. When sodium bicarbonate was extracted with DCM the sodium in sodium bicarbonate reacted with carboxylic acid functional group in Aspirin to form sodium acetylsalicylate salt.
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Generally, there are two ways in preparing a solution, one is by dissolving a weighed amount of solid in a required solvent and the other is by dilution of a concentrated solution into the desired concentration. In diluting concentrated solution, the concentration of the diluted solution can be determined by standardization. To standardize a solution, we will need to perform titration. In this ...
Therefore if DCM was to be extracted with HCL the sodium acetylsalicylate would not be formed and sodium acetylsalicylate would remain in the DCM layer therefore the percentage of Aspirin and the unknown component would be higher than expected. d. You neutralised sodium bicarbonate solution to pH 7 rather than pH 2. . 4. Acetanilide and phenacetin are not appreciably acidic paracetamol is stronger acid than water. What problem would you encounter if the unknown compound was Paracetamol rather than acetanilide or phenacetin, and you extracted the aspirin with 5% NaOH? Explain giving equations for relevant reactions.
Paracetamol has –OH functional group and aspirin has-COOH (carboxylic acid) functional group. Both these functional groups would react with Na when NaCHO^3 is added to paracetamol and aspirin. Therefore they would both produce sodium salts which would both move from the insoluble layer in DCM to the soluble aqueous layers making it difficult to separate the Paracetamol and Aspirin components. 5. Paracetamol is weaker acid than carbonic acid but aspirin is stronger acid than carbonic acid. Prepare a flow diagram like the one in this experiment, showing a procedure for separating a mixture of sucrose, aspirin and paracetamol.
