Experiment 2 Thin Layer Chromatography analysis of analgesic drugs
Miten Patel
Chemistry 3201
Date 2-2-2017
Objective: To Find the composition of a series of over the counter painkillers using TLC.
Chemical Equation: N/A
Chemical Mechanism: N/A
Safety Considerations:
• All Students must wear goggles when dealing with the chemicals in the lab, and wear gloves to protect their skin from the chemicals used.
• The capillary tubes are fragile and sharp. For clean-up, the chemicals can be disposed of down the drain.
Back ground
Thin layer chromatography In this lab, we were working with pain reliever drugs. Which we need to identify by TLC method. In chromatography, a partitioning occurs between a mobile phase and
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Which is going to be Aspirin and Acetaminophen.
3. Prepare a TLC chamber using a 250 ml clean and dry beaker. Then put a filter paper in beaker horizontally and add 15ml ethyl acetate containing 0.5% acetic acid. (The reason is put paper horizontally, when we put our alcohol in beaker so paper can stick with it). Cover the beaker.
4. Place the plate in TLC chamber and allow the solvent to run plate to about 1cm from the top. When solvent run above 1cm on plate take that plate out from chamber and drew a line with pencil.
5. Then see your plate in UV lights (short wavelength) and circle all what you see in UV lights.
6. Place your plate in iodine chamber for 2 to 3 minutes then make sure all your circle and calculate retention factor (Rf) value with the help of equation above. And stick plates in our notebook.
Rf = Distance traveled by the sample (cm) Distance traveled by the solvent (cm)
For unknown
7. I have no 54 unknown sample to identify which is in solid form. In the given sample add 50/50 mixture of ethanol and methylene chloride. Stair it and mix it well. Allow some time to mix it well so insoluble fraction can dissolved properly.
8. Spot the mixture by using capillary on TLC plate like we did on the first part. Prepare TLC chamber with filter paper and ethyl acetate. Put your TLC plate in chamber and allow it to run plate above 1cm at top. Mark the position.
9. Check your plate in UV lights. Circle all spot calculate the value of Rf with help of
The goal of this experiment was to find out active chemical components in Anacin and Tylenol, using Thin Layer Chromatography technique. This technique uses the difference in the intermolecular forcer and polarity to separate mixtures. Comparing Rf values were then used to determine the active chemical components in the two analgesics. The overall result was that Acetaminophen exists in Tylenol and Acetylsalicylic Acid exists in Anacin.
Step 4: Place the test tubes into separate coffee cups to maintain the upward position. Add 2 mls of the catalase solution to each of the test tubes and then place tubes1, 2, and 3 in the conditions described above. For test tube 4, fill the coffee mug half full of boiling
The first step that needed to be done in this experiment was adding hydrochloric acid (HCl)
The objective of this extraction experiment was to achieve a comprehensive understanding, as well as master the practice, of the technique of separating various individual components of a compound.
Add to this 5 drops of pH 4 buffer solution * Measure out 2 cm³ starch solution * Start stopclock and leave for 1 minute * Measure out 1 cm³ amylase and place in second corvette * Add to this 2 cm³ distilled water *
First, obtain a SpectroVis Plus device and connect with its corresponding LabQuest2 device. You need to calibrate by turning on the machine, allow the inner lamp to start heating up, and prepping a blank in the process. Obtain a dry cuvette, fill it with distilled water, and place into the SpectroVis plus device. Before doing so, be sure to wipe the outside of the cuvette with a Kimwipe to clean off any fingerprints that might be present. Fingerprints will skew with the calibration. Once the device notifies you that calibration is complete, click okay and prep for the next part of the lab.
4.Measure 35mL of warm water and add them into each of the 4 test tubes at about roughly the same time. It is essential that the water is warm. Do not seal the test tube.
Wash (swirl and shake) the organic layer with one 10-mL portion of water and again drain the lower aqueous layer. Transfer the organic layer to a small, dry Erlenmeyer flask by pouring it from the top of the separatory funnel. Dry the crude t-pentyl chloride over 1.01 g of anhydrous calcium chloride until it is clear (see Technique 12, Section 12.9). Swirl the alkyl halide with the drying agent to aid the drying.
Caution – Hydrochloric acid is corrosive to eyes, skin and clothes. Wearing a lab apron, rubber gloves, goggles, and a face shield is essential. Rinse any spills on skin or clothing with plenty of cold water. Clean up spills immediately – ask your instructor for help.
AIM: To extract codeine and paracetamol from its tablet by solvent extraction and tentatively identify in comparison to standards using Thin Layer Chromatography.
1 ml of water should be added to the first test tube and make a note. In the second test tube, 1 ml of methyl alcohol should be added. In the third test tube, 1 ml of hexane must be added. Lastly, the fourth test tube will be a control.
Submerge the graduated cylinder in the plastic tub so that it is completely filled with water. Hold the open end of the graduated cylinder and move it vertically upside-down where the open end of the graduated cylinder is still submerged in the plastic tub. Clamp the graduated cylinder the ring stand of the lab table to keep it in place. perforate a hole in the top of the rubber cork for the solution container. Cut a straw the length of about four inches. place the straw inside of the rubber cork hole. Set up your timer for two minutes.
2. Add about 20 mL of distilled water and stir the mixture with a glass stirring rod to dissolve the sample. There may be a small amount of insoluble residue. If your sample does not dissolve completely, remove the insoluble material by filtration.
3. Use a sterile pipette to transfer 0.1 ml of each dilution on to a MacConkey agar plate.
4. Spot the solution on a TLC plate and check with UV light to see