Opioids CWE - Something crystallized out after I cooled

[CrimpJiggler]

I did a CWE on tablets containing codeine phosphate and APAP. I tried something different this time, to ensure that all codeine got dissolved, I dissolved the powder in boiling water and stirred like mad. I put it in the fridge to allow it to cool down. I came back and the liquid looks fairly clear but there are white crystals stuck to the walls of the glass (I did it in a pint glass). I scraped it off with a butter knife and the crystals were hard and brittle, not at all like the fine powder I'm used to dealing with when doing CWEs. This is the first time I've seen something like this happen. I could literally filter these crystals out with a sieve. Have any of you seen this happen before? Theres no way codeine phosphate would crystallize out of water like that so this seems like a superior way to do CWEs. A large amount of APAP gets dissolved in the boiling water but due to its steep solubility curve, the majority of it crystallizes back out and forms nice big, easy to filter APAP crystals.

EDIT: I'm a bit reluctant to go ahead with this CWE because maybe the heat provided the energy needed for a reaction to occur between one of the APIs and/or excipients. Then again I know what types of reactions could be possible and I would know if their products were present.

Also: In case anyone decides to further propagate the myth on this thread, I'll say this now. Codeine (or any other common opiate) will NOT decompose under temperatures as low as 100C. Thats some kind of wives tale that has gotten out of control. Codeine melts at 150C. I can't find a decent source for this but according to this page:
http://www.wolframalpha.com/entities/chemicals/codeine_phosphate/lg/ue/ij/
codeine phosphate melts at 220C. Its about time we killed this silly myth. Next time you're wondering what temperature a compound decomposes at, look at its MSDS.

 

[rickolasnice]

Yeah i've had this when i left it in the fridge too long (the back of my fridge is cold enough to freeze things - but it wasn't ice)..

I wouldn't trust it.. i just heated it up again, stirred, and put it back in the fridge for less time..

I always use hottish water to do my CWEs it shouldn't cause any problems.. I've even once put a dihydrocodeine solution (after filtering APAP out) in a dish on a saucepan of boiling water.. i didn't trust what i was left with so scraped the powder / crystal lookin stuff into water and just did the CWE again.. didn't cause me any problems and the dihydrocodeine still worked..

 

[CrimpJiggler]

I'm gonna go ahead and do the CWE and weigh the residue to make sure enough of the APAP has been filtered out. Theres always the possibility that the solution is supersaturated with APAP. If some crystals have formed, then its not supersaturated though. Solutions only remain supersaturated when there are no nucleation sites for crystals to form.

 

[Coolwhip]

Why use hot water at all? The only thing that matters is the temp while filtering. Do you just like dissolving/precipitating APAP, or is adding extra unnecessary steps part of your OCD?

Making sure you dissolve all the fillers that you can,(before making them again fall out of solution) and dissolving all the codeine you can aren't the same.

My point is, in trying to 'at some point' have 100% of the codeine dissolved you are probably going to spend WAY more time and be less successful by heating and cooling your solution...than by just allowing the codeine to sit/stir in the already cold solution a little longer.

 

[rickolasnice]

^ Takes fuckin ages to dissolve the pills if you simply add them to cold water and stir.. unless you crush them up (which also takes fuckin ages)

There is no harm in using hottish water to dissolve the pills if you then cool the solution enough.. How will this take longer? Put pills in glass.. use the hot tap to add a little water (i have one of those taps u can vary the temperature), stir for about 1 min or less.. put in fridge.. take out and filter.

What unnecessary "extra steps" am i taking, exactly.. i count the same amount.. minus 1.

 

[Swim 1211]

Why not crush the pills first?? I don't see what's difficult or time consuming about doing that??

 

[docs - docs]

Here's something i read in the Great Textbook of Excipients... I'm going to paraphrase since I dont remember the exact title of the book or the exact line:

"IR pills are designed to dissolve in a MINIMUM of available solvent (water). The capillary action of the _____ allows for moisture to be drawn into the pill causing it to swell and break apart."

See, pills don't really dissolve, they have in them things like cellulose that are meant to force the pill to break apart in the presence of moisture. For whatever reason, when you add more water it takes longer for this too happen. From what I've seen, if you're having trouble with these pills dissolving, just barely cover them with water and let them sit undisturbed for 10 mins or so.

I've seen it work more than not, but less with APAP than ASA

 

[RobotRipping]

i use hot water from a tap not too hot but just enough to dissolve the pills as described above. I used to use a coffee grinder, i find little difference. I use the freezer for about 20-25 minutes just before the apap freezes and i stir it a few times while it's in the freezer, if i get it just right the apap will crystallize and i'm left with easy to filter codeine water. I'm not sure about how much is lost like this but i get very clear and bitter as fuck liquid every time. I use 2 coffee filters with paper towel, in the next batch ill squeeze the shit out of the filters and refilter it with more pills.

 

[sekio]

Hot water won't cause any such "reactions" between the API's/binders. Your crystals are likely just APAP.

 

[rickolasnice]

Why not crush the pills first?? I don't see what's difficult or time consuming about doing that??

Answer a question with a question: Why crush the pills?

I dunno if the pills round my way are different but all i have to crush them is 2 spoons.. and it takes forever.