This is my first post here so I hope it's in the right section. I have a major issue here with extraction of pseudo from OTC tablets. I went with the "Full turps cure" method and modifies it to include an A/B extraction at the end.
The ingredients in these pills are as follows:
Pseudoephedrine HCl - 60mg
Acetaminophen - 500mg
Inactives:
Corn starch
Crospovidone
Magnesium stearate
Stearic acid
POVIDONE
Microcrystalline cellulose
Silicon dioxide
4 boxes of 24 caplets was used (5.760g pseudo)
Now because these have so much acetaminophen, first i did 3 acetone boils to remove acetaminophen and any other acetone soluble ingredients. Carefully decanted and set aside the spent solvent to distill back later for recycling. I did this first as in previous experiences acetaminophen really fucks up the rest of the procedures.
Now what I should have done next was the first step of the turns cure, and soak in hot xylene/mineral turps for 12hrs. But I foolishly skipped this step due to the stink of these solvents. So I proceeded to do the alcohol extractions. Twice with 99% IPA, and once with methanol. Upon evaporation of alc I got a measly 0.20g of extract!!! This really confused me. So that's why I added in the A/B extraction to see if that could extract the goods. I put the dried powder pill mass into a 150mL flask and with distilled water shook the hell out of it for about 10 minutes then let settle for 30mins and filtered tye solution, then when all the water passed thru filter, making sure it was not containing sediment, I dried the pill mass in the filter, and repeated this 3 or 4 times and combined the water extracts.
This is where things got messy.
I basified the solution with NaOH, and I immediately saw the pseudo freebase float uo to the top, which was a wonderful sign, but within minutes quickly disappeared! So I added xylene to extract tge freebase, added salt, added more naoh then shook the solution just to get an absolutely HORRIBLE emulsion that I have had hell trying to deal with. I tried adding more salt until it was saturated, more naoh, but nothing has worked! I even tried concentrated hydrogen peroxide (~20-25%) which almost seemed like it was helping, but I barely had much left and used it all up, still to no avail. So I went ahead and separated tye layers, and took the xylene pulls, washed with dH20 separated, then with acidification H20 with Hcl, evaporated my water (and hopefully pseudo hcl) and got a measly 0.21g of crude pseudo. Totalling 0.41g of pseudo from 5.76g I put in.
I'm assuming tye pseudo is still in the emulsion water. Any help please send thank you!
The ingredients in these pills are as follows:
Pseudoephedrine HCl - 60mg
Acetaminophen - 500mg
Inactives:
Corn starch
Crospovidone
Magnesium stearate
Stearic acid
POVIDONE
Microcrystalline cellulose
Silicon dioxide
4 boxes of 24 caplets was used (5.760g pseudo)
Now because these have so much acetaminophen, first i did 3 acetone boils to remove acetaminophen and any other acetone soluble ingredients. Carefully decanted and set aside the spent solvent to distill back later for recycling. I did this first as in previous experiences acetaminophen really fucks up the rest of the procedures.
Now what I should have done next was the first step of the turns cure, and soak in hot xylene/mineral turps for 12hrs. But I foolishly skipped this step due to the stink of these solvents. So I proceeded to do the alcohol extractions. Twice with 99% IPA, and once with methanol. Upon evaporation of alc I got a measly 0.20g of extract!!! This really confused me. So that's why I added in the A/B extraction to see if that could extract the goods. I put the dried powder pill mass into a 150mL flask and with distilled water shook the hell out of it for about 10 minutes then let settle for 30mins and filtered tye solution, then when all the water passed thru filter, making sure it was not containing sediment, I dried the pill mass in the filter, and repeated this 3 or 4 times and combined the water extracts.
This is where things got messy.
I basified the solution with NaOH, and I immediately saw the pseudo freebase float uo to the top, which was a wonderful sign, but within minutes quickly disappeared! So I added xylene to extract tge freebase, added salt, added more naoh then shook the solution just to get an absolutely HORRIBLE emulsion that I have had hell trying to deal with. I tried adding more salt until it was saturated, more naoh, but nothing has worked! I even tried concentrated hydrogen peroxide (~20-25%) which almost seemed like it was helping, but I barely had much left and used it all up, still to no avail. So I went ahead and separated tye layers, and took the xylene pulls, washed with dH20 separated, then with acidification H20 with Hcl, evaporated my water (and hopefully pseudo hcl) and got a measly 0.21g of crude pseudo. Totalling 0.41g of pseudo from 5.76g I put in.
I'm assuming tye pseudo is still in the emulsion water. Any help please send thank you!