Hello,
I know many of you love the "Agent Lemon" or 'Dual Phase Acid-Base" extraction methods, but why have so many steps and potential contamination? Why not keep it as simple as possible with the least amount of variables and the highest yield..
After reading the whole DXM faq, searching many threads on here & elsewhere an idea came to my head, "DXM Extraction by centrifugation". MODS move this to appropriate section if required.
So according to the dxm faq :
If you want to use the precipitation method, all you have to do is add sodium hydroxide to the cough formula as described above, until the DXM precipitates out. Let it stand (or centrifuge it), and filter. The (very fine) powder that hopefully was caught by the filter paper is the DXM free base.
This is my proposed (and untested) new and improved method (I would like some help in some aspects, please comment)
The Materials:
-DXM-containing cough syrup. (30mg/10ml HBr 200ML Robo I'd use)
=Sodium Hydroxide (NAOH) (I have Pure reagent grade granules)
The Equipment: (I know most wont have this)
=High Speed Centrifuge (Up to 5000RPM, Not the small tabletop ones!)
=50ml Plastic Tube with lid
=Beaker/Flask/Bottle able to hold at least 1L
Details
1. Transfer the syrup to a container of choice (1L minimum)
2. Add (5 grams?) of NaOH granules to the syrup and stir/shake until a milky/clody solution is formed and white precipiate is visible. Keep adding NAOH until precipiate is fully insoluble. (Ok this is where I need the community's help, does anyone know the approximate amount required to fully precipitate the DXM? Or is it simply make the solution reach ph14..?)
3. Pour a maximum of 50ml of this solution to the Plastic Tube and balance the centrifuge with another tube of 50mls water/etc.
4. Spin down at 2000 RPM for 5mins (Unsure of speed and time atm, 2000 @ 5mins might be sufficient)
5. A tiny pellet should be visible, discard the supernatant by any means (Aspiration preffered) and repeat steps 3&4 until no solution is left, you should notice the pellet getting larger each time as more DXM is being collected.
6. -Optional - Wash the pellet by 'mixing' it with 5mls or less of dH20 (Filtered water) to remove any lingering NaOH,etc and then spin down again to remove the water Solubility of DXM in water is 1.5 g/100 mL at 25 C so loss will be minimal.
7. Transfer the pellet (to a smaller tube/eppendorf) and dry by leaving it in the air or (If available) a heat block at 50-80C as Dextromethorphan's melting point is 122-124C. You could also leave in the same 50ml tube for no loss!
8. You should now have pure DXM Freebase powder, with minimal if any contaminants such as Naptha/Ammonia,etc. If you have a micro scale why not weigh the sample, for a 200ml bottle with 30mg/10ml, theoretically 600mg but perhaps 550mg+ due to some loss.
As this is untestested, a few things come to mind which ill cover here.
1. Spin down pure syrup and see if any pellet forms.
2. Spin a concentrated aqueous solution of NAOH and see if any pellet forms.
If both of these show no pellet, we can be quite assured the only compound in the pellet when performing the actual extraction is in fact only DXM!
If anyone has performed something similar/has any comments/suggestions whatsoever PLEASE comment so this method can be perfected =)
I know many of you love the "Agent Lemon" or 'Dual Phase Acid-Base" extraction methods, but why have so many steps and potential contamination? Why not keep it as simple as possible with the least amount of variables and the highest yield..
After reading the whole DXM faq, searching many threads on here & elsewhere an idea came to my head, "DXM Extraction by centrifugation". MODS move this to appropriate section if required.
So according to the dxm faq :
If you want to use the precipitation method, all you have to do is add sodium hydroxide to the cough formula as described above, until the DXM precipitates out. Let it stand (or centrifuge it), and filter. The (very fine) powder that hopefully was caught by the filter paper is the DXM free base.
This is my proposed (and untested) new and improved method (I would like some help in some aspects, please comment)
The Materials:
-DXM-containing cough syrup. (30mg/10ml HBr 200ML Robo I'd use)
=Sodium Hydroxide (NAOH) (I have Pure reagent grade granules)
The Equipment: (I know most wont have this)
=High Speed Centrifuge (Up to 5000RPM, Not the small tabletop ones!)
=50ml Plastic Tube with lid
=Beaker/Flask/Bottle able to hold at least 1L
Details
1. Transfer the syrup to a container of choice (1L minimum)
2. Add (5 grams?) of NaOH granules to the syrup and stir/shake until a milky/clody solution is formed and white precipiate is visible. Keep adding NAOH until precipiate is fully insoluble. (Ok this is where I need the community's help, does anyone know the approximate amount required to fully precipitate the DXM? Or is it simply make the solution reach ph14..?)
3. Pour a maximum of 50ml of this solution to the Plastic Tube and balance the centrifuge with another tube of 50mls water/etc.
4. Spin down at 2000 RPM for 5mins (Unsure of speed and time atm, 2000 @ 5mins might be sufficient)
5. A tiny pellet should be visible, discard the supernatant by any means (Aspiration preffered) and repeat steps 3&4 until no solution is left, you should notice the pellet getting larger each time as more DXM is being collected.
6. -Optional - Wash the pellet by 'mixing' it with 5mls or less of dH20 (Filtered water) to remove any lingering NaOH,etc and then spin down again to remove the water Solubility of DXM in water is 1.5 g/100 mL at 25 C so loss will be minimal.
7. Transfer the pellet (to a smaller tube/eppendorf) and dry by leaving it in the air or (If available) a heat block at 50-80C as Dextromethorphan's melting point is 122-124C. You could also leave in the same 50ml tube for no loss!
8. You should now have pure DXM Freebase powder, with minimal if any contaminants such as Naptha/Ammonia,etc. If you have a micro scale why not weigh the sample, for a 200ml bottle with 30mg/10ml, theoretically 600mg but perhaps 550mg+ due to some loss.
As this is untestested, a few things come to mind which ill cover here.
1. Spin down pure syrup and see if any pellet forms.
2. Spin a concentrated aqueous solution of NAOH and see if any pellet forms.
If both of these show no pellet, we can be quite assured the only compound in the pellet when performing the actual extraction is in fact only DXM!
If anyone has performed something similar/has any comments/suggestions whatsoever PLEASE comment so this method can be perfected =)
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