Sasha Thiel
09.10.2012
CH203 Lab
Experiment 1: Isolation of the Active Ingredient in an Analgesic Drug
Pre-Lab:
A. Least accurate to most accurate 1. Beakers (5ml markings) 2. 10ml graduated cylinder (0.1 markings) 3. 5ml vials (0.1 and 0.3 markings) 4. 1ml plastic pipets (0.1 ml markings) 5. 1ml syringes (0.1 ml markings) 6. 1ml graduated volumetric pipets (0.01 ml markings) B. A 1ml graduated volumetric pipet is the best to use if you want 0.15 ml of reactant C. 1ml plastic pipets (used 2 times) are best to use when you want 2 ml of solvent
Safety Hazards: 1. Methanol is flammable and toxic. Don’t breathe it in or drink it. 2. All organic waste goes in the waste containers and not
…show more content…
(Note: Ibuprofen is slightly sticky even when dry) 6. Weigh watch glass now and determine weight of active ingredient 7. Calculate weight % recovery using weight from label 8. Crush crystals into powder with a stirring rod and use a melting point device to determine the melting point of your active ingredient. 9. Record the melting point. Watch for sweating or shrinkage 10. Place product in a small vial and label it for the professor.
Observation:
My analgesic
Use a glass beaker to pour an adequate amount of the liquid substance and use the pipette from the glass beaker.
The mixture was transferred to an ice bath to crystallize the product, after which the product was collected by vacuum filtration on a Hirsch funnel, washing the flask with small aliquots of cold xylene and pouring the solution over the crystals, allowing the vacuum to thoroughly dry the product. Additional drying was achieved by transferring the product to filter paper and pressing the crystals to remove any excess moisture. The product was then weighed and a melting point determined. A comparative TLC was run in Hexanes:Ethyl Acetate solvent against maleic anhydride to verify the purity of the
An automatic pipet was used to measure 0.450 mL water and 0.165 mL acetic anhydride and was added to the conical vial. A spin vane was placed into the vial and an air condenser was attached.
16) Heat some of the hexane to boiling and place the solid to be crystallized into an Erlenmeyer flask.
The product was then suspended in 2 ml of water with a stir rod in a 50 ml Erlenmeyer flask and heated to boiling. Water was added in one milliliter increments until all the product was dissolved (18 ml added total). The saturated solution was allowed to slowly cool, and gradual white crystal formation was observed. Recrystallized product was collected once more by suction filtration with the Hirsch funnel once crystallization ceased. Collected product dried on a watch glass for a week, weighed 0.14 g (1.2 mmol), and the melting point was 139°-141°
Sodium bicarbonate has a molar mass of 84.0 g/mol. It has a melting point of 50°C and can be an irritant.
* By using the dropper and measuring cylinder, 7 ml sodium carbonate solution was added to the test tube
• Serially dilute the 4 mg/ml solution with buffer A to make working solutions of 400 µg/ml and 40 µg/ml.
9. Each of the other solutions is already approximately 0.1 M. With these solutions you can pour a small
The correct syringe is used to place 10 cm3 of the first glucose solution into the boiling tube.
Tube 4 now should only have crude solid in the tube and it is then weighed. The tube is placed into a 50℃ water bath and then approximately 0.5 -1 ml of methanol is added, as well as H2O until the solution gets cloudy, once the solution is dissolved it is cooled to room temperature and then iced. The crystals are then collected using a Hirsh funnel. Next a small amount (~ 0.1g) of the crystals are placed into a melting point tube and placed into the melting point machine to record the unknown neutral substances melting point.
Components containing caffeine were composed into stock solutions. These solutions were diluted to 1: 10 substance: mobile phase. A stock solution of caffeine was diluted 1:50. A sequence of diluted caffeine solutions were prepared for use as a standard (ppm): 1, 2, 4, and 10. Solutions of acetaminophen, acetylsalicylic acid, and Goody’s Powder were developed to differentiate chromatographic peaks observed. These solutions were subjected to HPLC for examination of the observed peak area and retention time for the set of compounds. Comparison of retention time allowed for the differentiation of peaks observed. The peak area obtained was utilized to determine the relative concentration of caffeine present in Goody’s Powder based on the relationship obtained in the standard. The content of caffeine present in Goody’s Powder by percent weight was identified.
PRACTICAL REPORT ON THE ISOLATION AND IDENTIFICATION OF CODEINE AND PARACETAMOLPRACTICAL REPORT ON THE ISOLATION AND IDENTIFICATION OF CODEINE AND PARACETAMOL
3. Use a sterile pipette to transfer 0.1 ml of each dilution on to a MacConkey agar plate.
Analgesics: NSAIDS, Opioids - Can be administered PO or parenterally - Side effects incl. constipation - Danger of infection Thermal application: Heat/cold - Heat: Reduces pain, Increases healing - Cold: Reduces swelling, promotes numbing - Thermal application applies comfort. - Too hot for patient, risks of burning - Too cold for patient, risks of frostbite Massage - Reduce inflammation - Reduce fluid buildup - Reduce muscle tension and promote comfort - Distraction from pain - Invasive -