Reduction of Cold Water Extraction of Nurofen Plus

[doctorheisenberg]

I've spent the last few days scouring over the posts on this site and others. There are thousands on harm reduction and cold water extraction (CWE) out there, however most are horrendously amateur and written by teens who've gained access to the medicine cabinet.

I have recently CWE'd a batch of nurofen plus (500mg of ibuprofen / 12.8 mg of codeine phosphate) and used a multi-filtration method of CWE to ensure the final product is clean. There is a slight cloud to the product, and a bitter taste, yet the stranger behaviour is the adulterant of unknown origin that on evaporation yields a flake instead of a powder.

Very few people seem to have the time to properly filter in their CWE, and even less go through the bother of reduction of the finished product, but as a chronic pain sufferer with a non-metabolization through hepatic function I've reluctantly found insufflation is the only method of action that works for me. Previously I've only had effects from mK-receptor opiod agonists, but in this case I believe codeine is a Mu but it definitely had some effect.

The ibuprofen is a very unwanted element, just as paracetemol (acetominophen (sp?) / apap) is in nations outside Australia / NZ where they can't get 72 packs of nurofen plus, and it really does seem to filter out quite well if you follow a proper CWE extraction method not written by an illiterate twelve year old, but fucked if I can find any place online that actually addresses evaporation or reduction.

So, I've turned to this forum, specifically advanced drug discussion in hopes I can get an enlightened response as opposed to "i jooz moy sox to filter eet".

I know in ... well, this forum doesn't allow discussion of synthesis of drugs, but (hoping this doesn't count as a reference) I'm aware that in meth cooking the product is washed in various boiling solvents. I was wondering if a solvent wash of any form would remove the residue that's causing the finished product to flake instead of powder? I sprayed isopropyl on a batch that yielded a bit of burning, and the resultant scum line where the iso evaporated off makes me think that iso will melt it, but the problem is I'm unsure if the iso is also destroying the codeine molecules present or adulterating them in any way.

I figured I'd turn to this forum as a last ditch effort rather than sampling the cleaned up codeine myself after various solvents (I'm unsure whether it's even safe to insufflate solvent washed meds?). One alternative I was pondering was using bicarbonate of soda as a base for the codeine molecules to bind to, I'm unsure whether that's a way around the flake or not, but I'm very open to suggestions.

Please, if you're not a regular on the ADD forum, please, please, please don't derail this with how you like to filter things with your socks, or asking about CWE in general, there's a metric tonne of CWE FAQ's and info out there, but nothing about evaporation to a clean product, I'm talking stuff from sticking it up your butt through to making codeine kool aid, so google to your hearts content but I want to deal purely with evaporation, molecular decay, cleaning the final product, and whatever this mystery filler or adulterant is in my meds.

Thanks in advance to any and all chem geeks who reply. Harm reduction IS a noble cause, and harm reduction is the reason I CWE this stuff and am using it instead of the oxycodone I've been perscribed (perilous path I've been down too many times, so sticking with something OTC).

 

[TheMiddleWay]

Cannot part the full source document, but I don't think filtering stuff is synthesis since it's harm reduction. Please remove if I'm wrong...

Several packets of tablets, sufficient to yield about 2 g of codeine, are crushed and mixed with water. The mixture is filtered using a filter pump, Buchner funnel and side-arm flask, to remove tablet binding agents, diluents and other excipients. The aqueous filtrate is poured into a separating funnel and sodium hydroxide solution added to make the solution strongly alkaline. This is then extracted with chloroform (about 50 ml). The chloroform layer is drained off and evaporated to dryness using gentle heating (often on a domestic stove). The aqueous layer containing aspirin and paracetamol is discarded. The codeine base is recovered as a white crystalline solid.

 

[pete_gasparino]

You will do more harm than good with any sort of organic solvent extraction, in this context - without certain glassware and knowledge of its use you are more likely to ingest harmful compounds (for example, isopropanol).

yet the stranger behaviour is the adulterant of unknown origin that on evaporation yields a flake instead of a powder.

What makes you think there's an adulterant?

There are many reasons why an evaporated, solid product can appear flaky rather than a powder: lots of evaporated salts do appear as flakes. It depends how the solvent was evaporated: ie the oven temperature (or was it outside? or with a hairdryer?), the rate of evaporation, the dish on which you evaporated it, etc etc.

I sprayed isopropyl on a batch that yielded a bit of burning, and the resultant scum line where the iso evaporated off makes me think that iso will melt it, but the problem is I'm unsure if the iso is also destroying the codeine molecules present or adulterating them in any way.

I don't quite know what you mean here, but do not spray ispropanol on anything you're about to ingest.

Low levels of unwanted contaminants (meaning, unwanted materials - consider all the materials in the pills incluing inactive ingredients that have the same solubility as codeine) will do little harm, and the time and equipment required to remove them is not worth your time.

Mucking about with isopropanol or chloroform will increase the potential harm of this process beyond what any pill binding contaminant could do.

 

[doctorheisenberg]

I iso wash the glassware between use to void it of any contaminants and moisture and evaporate it then steam clean it to avoid any cross contamination between CWE's. TheMiddleWay's method makes sense, however without access to a lab or chloro the closest thing I'd be able to get my hands on would be ether, and even that's always tainted with other hydrocarbons. I'm limited to industrial type solvents, and can make any anhydrous as required, but I'm thoroughly at a loss as to what would eat the yield or what would retain it out of them.

Pete, you're right with the flake, I don't have any knowledge of whether that's what codeine phosphate looks like in it's natural state, but there are many references to 'evaporating it to a powder', which never go into detail about how the evaporation is done, many do it under slight heat on an evap dish, some put it in the sun or otherwise destroy their yield in the process, I do the former and keep the heat very light.

The fact I filter it a half dozen times more than neccessary makes me think whatever it is, if it's not it's natural state, it's something that is soluable and filterable in exactly the same way as the codeine. I have however done some reading up on splitting Nurofen plus, which seems to minimise the gack and ibuprofen in the solution, and am CWE'ing a batch of that now. I've also obtained perscription paracetemol and codeine (there's few medications in Australia that aren't ibuprofen and codeine, so I'm still very interested in CWE and evap of it for availability) and will be performing the same exacting CWE to see what the codeine phosphate looks like from THAT evaporated under the same method.

The heating element I use to evap is set to no more than 30C, I reduce that as the mass of solution decreases to make it as slow a process as possible. The iso spray onto the yield that I mentioned was done on burnt material (I couldn't monitor it due to IRL obligations) so it was already wrecked, but I wanted to see whether whatever caused the flake was soluable in isopropyl alcohol, which it appeared to be; but again I don't know whether the codeine was in the iso mix or the powder left behind, and it's not something I want to test with my nose.

Thank you both for replying, I hope this makes more sense, and I actually feel as though I'm finally heading towards some answers, after so much time pissing in the wind it's actually very refreshing!

 

[pete_gasparino]

I iso wash the glassware between use to void it of any contaminants and moisture and evaporate it then steam clean it to avoid any cross contamination between CWE's.

Whether you're removing contaminants with isopropanol, depends on if the contaminants are soluble in that solvent. This seems an extraordinary amount of effort, for no particular reason:
for example, why did you choose the solvent you did? Why does the glassware need to be dry? Wouldn't you do a final wash with acetone if you wanted dry glassware? Why are you steam cleaning it? What makes you think that these methods are going to result in a piece of glassware any freer from contaminants than simply, say, washing vigorously several times with water, then detergent, then water?

What I am saying is, it seems as though you haven't examined the utility of each step, in this whole process. More steps doesn't mean a cleaner product.

TheMiddleWay's method makes sense, however without access to a lab or chloro the closest thing I'd be able to get my hands on would be ether, and even that's always tainted with other hydrocarbons. I'm limited to industrial type solvents, and can make any anhydrous as required, but I'm thoroughly at a loss as to what would eat the yield or what would retain it out of them.

Again, I just fail to see the utility of this. I can see all sorts of scenarios where you end up at best losing your product, at worst hurting yourself.
I think you are making this process much more complicated than it needs to be.

Do you have a Buchner funnel and flask? Do you have a vacuum pump, so that you can use the Buchner apparatus? Do you have a separatory funnel? Are you aware, for example, that chloroform, diethyl ether, and isopropanol all have different abilities to dissolve different substances? That diethyl ether is remarkably flammable, and best used in a hume food? What's the point? You don't even know the product is contaminated such that liquid-liquid extraction as described, would clean it.

Pete, you're right with the flake, I don't have any knowledge of whether that's what codeine phosphate looks like in it's natural state, but there are many references to 'evaporating it to a powder', which never go into detail about how the evaporation is done, many do it under slight heat on an evap dish, some put it in the sun or otherwise destroy their yield in the process, I do the former and keep the heat very light.

The fact I filter it a half dozen times more than neccessary makes me think whatever it is, if it's not it's natural state, it's something that is soluable and filterable in exactly the same way as the codeine.

I'm no crystallographer, but I've done plenty of evaporations of salts on watchglasses, and lots of those appeared flaky. I can't explain in detail the reason why your method of evaporation results in this morphology but jumping to the conclusion that some contaminant (aside from those that are beyond reasonable capacity to remove) is present and causing this flaking, seems strange.

Filtering more often will not remove soluble contaminants, only insoluble ones. If something is soluble, it flows right on through the filter, along with the codeine.

I have however done some reading up on splitting Nurofen plus, which seems to minimise the gack and ibuprofen in the solution, and am CWE'ing a batch of that now. I've also obtained perscription paracetemol and codeine (there's few medications in Australia that aren't ibuprofen and codeine, so I'm still very interested in CWE and evap of it for availability) and will be performing the same exacting CWE to see what the codeine phosphate looks like from THAT evaporated under the same method.

Chemists Own sell a brand of strong pain killer I believe, which contain 10mg of codeine and 500mg of paracetemol. They are yellow tablets. Nurofen isn't the only game in town, and actually, probably put more fillers and binding agents into their capsules (I presume because of the shape of the capsule, the texture, and that they are suspending ibuprofen and codeine phosphate in a homogenised matrix).

Filtering several times is a good idea to remove paracetemol, but you don't know if you're removing any other undesired products - or if it's even possible. As to the contaminant: you could have your final sample instrumentally analysed, but I'm not sure it's legal to have unadulterated codeine in your possession, without a prescription :

The heating element I use to evap is set to no more than 30C, I reduce that as the mass of solution decreases to make it as slow a process as possible. The iso spray onto the yield that I mentioned was done on burnt material (I couldn't monitor it due to IRL obligations) so it was already wrecked, but I wanted to see whether whatever caused the flake was soluable in isopropyl alcohol, which it appeared to be; but again I don't know whether the codeine was in the iso mix or the powder left behind, and it's not something I want to test with my nose.

Thank you both for replying, I hope this makes more sense, and I actually feel as though I'm finally heading towards some answers, after so much time pissing in the wind it's actually very refreshing!

If you are intent on obtaining a pure product: find out each compound contained in the pill (from chalk/filler, binder, the wrap, and whatever the hell else they put in). If all but codeine are soluble in some solvent, go ahead and do a liquid-liquid extraction! But you'll find some will have precisely the same solubility as codeine. Are you then in the position, and do you have the inclination to move onto more difficult separation methods, like chromatography?

It seems to me, unnecessary, and probably futile.

 

[doctorheisenberg]

Obtaining a powder, rather than soapy flakes that cannot be ground into a fine powder, is the entire purpose. So whatever lengths I have to go to to obtain a clean powder product for consumption that avoids hepatic processing will be the lengths to which I'll go to. Surely it isn't that complex, and that there is material out there covering N+ CWE and evap?

Paracetemol and codeine is CWEing, so I have yet to examine the yield. But if it is also a soapy flake I'll be lost how to proceed. Tbh, I'd rather insufflate remnants of ibuprofen (although my filtration is clean enough to avoid that, but just an 'if') than APAP any day. The codeine flakes, as fine as I can attempt to grind them (which isn't) already cause rather serious discomfort.

 

[ebola?]

Honestly, codeine is kind of a high dose substance to be insufflating in the first place. However, you could make a concentrated solution with water or saline to put in a saline nasal misting bottle.

ebola

 

[skillet]

Why not plug it (rectal) instead? Even if it's pure, insufflating it can't be good for your nose, and the drip must be horrific.

Or just use the oxy, just because codeine's OTC doesn't mean it's not addictive.

 

[doctorheisenberg]

That's one of the better suggestions I've seen yet, thank you Ebola, I may look into that! The only downside would be that the H2O would increase the mass and of the solution lessening the chance of molecules of the active ingredient absorbing / contacting the mucous membrane compared to dry powder.

I have, however, attempted to see if codeine works with me, given my natural (not a drug abuser, only recently had to rely on analgesics to survive after a series of mini strokes and a lot of random brain playing the pain game type thing (hemiplegic migraines)) tolerance to pain killers.

Prior to discovering oxycodone, I thought people were 'faking' somewhat the effects of OTC analgesics. After being put on a total of 63 medications all of which aside from Oxy yielded NO analgesic response, I'm desperate to find a substitute. I've even 'abused' some hectic pain meds like fenatyl to get some relief, yet none worked. I've found the only difference is that oxy works on the mk receptor.

I recently places my soapy codeine flakes into a cold coffee, they floated on the surface allowing me to get it down in one mouthful, and consumed 300 mg's, 15 minutes later after no effect I consumed the same dose, half an hour later after a tiny mild sensation of perhaps analgesia (I'm talking maybe one mouthful of a light beer worth of effect) I consumed another 600. The slight affect I felt faded within 30-60 minutes, so sadly I am wondering whether finding out how to obtain fine powder is even worthwhile. I've read that codeine isn't as potent nasally, but then again oxy works nasally but when swallowed has 1/10th the effect with me.

Sometimes I wish I lived in the US where doctors weren't pussies about perscribing pain meds, especially when most think you're fucking around when you say you had NO reaction to the analgesics they gave you. To get my doctor to perscribe after trying a good 20 or so pain meds in a matter of a week, I had to literally just say look, I can't afford this anymore, and I don't want to have to down a bottle of vodka a day (which is what kept me going) to not be going out of my mind in pain when I have my turns, and showed him the reciepts of the $$$ worth of expensive meds I'd been given and were wasted. He thought I was on a disability pension and was getting them for free. ._.

Anyway, just figured a bit of a 'why I'm asking' is in order so anyone reading this isn't hesitant thinking I'm going to peddle codeine as some half cocked party drug or some unconscionable thing. But thank you all to those who have replied, as I said earlier, it looks like I'm heading to finding an answer here.

 

[swilow]

I just use my socks to filter it, and then eat my socks.

 

[pofacedhoe]

I just use my socks to filter it, and then eat my socks.

lol

 

[TheMiddleWay]

I usually do that with shorts.

I eat my shorts.

OP,

If you haven't found relief with fentanyl I have a feeling codeine is like peeing on a freaking large fire.

 

[doctorheisenberg]

TheMiddleWay, you're probably quite right. So far only mK agonist opiods have had any noticable analgesic effect on me.

Whilst I live in a country with a good free medical / health system getting pain management even though the negative impacts on my life have left me house-bound for 3+ days a week (biggest insult to injury is I can handle pain really well, so when I say something is hurting, it is -really- bad, so I wish it were a case of me being a pussy) and reduced my sleeping hours to probably 4 per night in broken bursts. My business fell into decline to the point that I had to sell it, my relationship is suffering, and still getting a referral to a pain management clinic is like getting blood from a stone, because I'm in my mid thirties I'm 'too young' for oxycontin or other mk delayed release treatments according to Australian doctors; even though the pdf from the department of health would in this case direct them to put me on it as a trial, take me off it, and if an improvement is noted, return me to it.

This codeine extraction is my last ditch attempt before trying to obtain something through alternate means, and I don't really want to think about what the next step is after that should that fail.