Isolation of the Active Ingredient in an Analgesic Drug

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Isolation of the active ingredient in an Analgesic Drug from extraction, filtration and melting point.

Chm237

Abstract:

Acetaminaphen was crushed then extracted for the active ingredient by mixing it with methanol. Then separated from the binders by centrifugation and a filtration technique using a Pasteur pipet packed with alumina. The remaining solvent was then evaporated to yield the solid analgesic(.2295g, 45.9% yield) which was collected by filtration and tested for the purity of the drug by the melting point determination. The melting point was (135-142 C) compared to the literature melting point values for acetaminophen (169-171 C) the lower melting point show that their were still impurities in the isolated ingredient.

Procedure:

The acetaminophen (0.5395g) was crushed and added to a conical vial and was mixed with 2ml of methanol then shaken and let to sit till the undissolved particles settled to the bottom and transferred the liquid into a centrifuge tube using a filter-tip pipet. Repeating the process with an additional 2mL of methanol. The solvent was then centrifuged for 3 minutes until the mixture had settled into a supernatant liquid layer and a solid layer. Then in a prepared alumina column with 0.5 mL g of alumina 2mL of methanol was added to column and then the solution containing the drug. Followed by 1 mL of methanol through the top of the alumina. Half of the solution was then transferred into a small container. The remaining solvent was then evaporated in a preheated 50 C water bath and gentle air stream until 1 mL was left. The remaining solvent was then added and evaporated completely.

Then cooled to room temperature where crystals slowly formed. Then placed into an ice-bath where more white crystals started forming. After cooling for 10 min at 0 C the crystals were then scooped and placed onto a Hirsch funnel for 10 min. The dried sample was then weighed (.2295g,...
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