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Cold Water Extraction of codeine from over-the-counter analgesics

G.Patton

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Introduction

A Cold Water Extraction is a method used to separate compounds that are mixed together by using their difference of solubility in water. A Common example that this may be performed on is Vicoden (hydrocodone, Acetaminophen).

Why do people perform a CWE? Simple reason: they are taking large amounts of the medication in question for whatever reason to gain the effects/benefits of one active ingredient (e.g. hydrocodone), or taking this medication long-term in large amounts, however at the same time they are putting themselves at risk of physical harm through the ingestion of large amounts of the combo ingredient, e.g. acetaminophen. A cold water extraction is a simple way to separate the water soluble compound from the relatively non-water-soluble compounds we do not want, e.g. Hydrocodone or codeine will dissolve in room temperature water but acetaminophen won’t to the same extent, allowing us to easily separate them.
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In the UK there are two opioids available over-the-counter at pharmacies; codeine and dihydrocodeine. There are many branded and generic preparations of each, but UK law requires that over-the-counter opioid painkiller products must contain little opioid content in comparison to the larger fraction of the non-steroidal anti-inflammatory drug (NSAID).

In the United States and other countries, there are opioid pills available with a multitude of different opioids mixed in with NSAIDs. These include but are not limited to hydrocodone, codeine and oxycodone.

Codeine and paracetamol (co-codamol)
In the UK, the cheapest and most available preparation is the generic pack consisting of 32 tablets, each containing 8 mg codeine phosphate and 500 mg paracetamol, usually available from neighborhood pharmacies. A single box of 32 tablets will contain 256 mg codeine phosphate and a massively toxic 16 g of paracetamol in total. Doctors can offer co-codamol containing 15 mg or 30 mg of codeine phosphate per pill along with 500 mg paracetamol. There are several popular brands available in the UK which are priced higher but contain no extra codeine than their generic counterparts. There are also effervescent forms of the product, which are not desirable for extraction purposes due to the increased solubility of the paracetamol, and other contaminants included in high quantity such as sodium.

Codeine and ibuprofen
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There are many preparations of codeine and ibuprofen available over the counter in the UK. Perhaps most well known is Nurofen+, which contains 12.8 mg codeine phosphate and 200 mg ibuprofen per tablet and comes in packs of 12, 24 and 32. The largest pack size can yield up to 409.6 mg codeine phosphate and 6.4 g ibuprofen. There are generic versions available in some pharmacies, but these may have reduced codeine content and may not be much cheaper per mg.

Dihydrocodeine and paracetamol (co-dydramol)
Also, available in the UK is the branded product Paramol in pack sizes of 12, 24 and 32 tablets, each containing 7.46 mg dihydrocodeine tartrate and 500 mg paracetamol. The largest pack size contains 238.72 mg dihydrocodeine and 16 g of paracetamol in total. Doctors can offer higher strengths; 10 mg/20 mg/30 mg of dihydrocodeine, along with 500 mg paracetamol.

Oxycodone and various other NSAIDS

Oxycodone pills may be combined with ibuprofen, aspirin, acetaminophen, or naltrexone under various brand names in the United States.


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Codeine phosphate
Water-soluble;
Boiling Point: 462 ºC at 760 mm Hg;
Melting Point: 238-240 ºC;
Molecular Weight: 397.4 g/mole;
CAS Number: 52-28-8 (phosphate salt).


Each AC&C (Aspirin Codeine) pill used in this extraction contained:
  • 8 mg codeine phosphate (1.6 g codeine phosphate / 200ct)
  • 15 mg caffeine (3 g caffeine / 200ct)
  • 325 mg aspirin (75 g aspirin / 200ct)
  • 127 mg junk (25.4 g / 200ct)

Procedure:

Obtain a quantity of tablets containing codeine, check to see if they contain anything other than codeine, caffeine, Acetaminophen/Aspirin/Ibuprofen. If they do, and you don't know whether or not it will be a problem, your best bet is not to use them.

1. 200ct uncrushed AC&C added to 600 mL beaker (net 95 g). Hot water was added to 550 mL mark. Stirred 0.5 h with magnetic stirring (if you don't have automated stirring, just stir occasionally over a 15 min). Make sure the tablets dissolve completely. Some dissolve on contact with water, while others need some help dissolving by crushing them. Note: not all of the tablet will dissolve, there are water-insoluble fillers in the tablet and not all of the A/A will dissolve either(which is what we want).
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Solid aspirin and pill binders (bottom layer) and codeine containing solution (top layer).
2. Cooled in fridge for 4 h. 360 mL decanted to 2nd beaker. 190 mL left in sludge layer (65% of 1.6 g codeine extracted).

3. 200 ml hot water added to 600 mL beaker. Stirred 5 min. Cooled in fridge for 4 h. Decanted 200 ml to 2nd beaker (18% of 1.6 g codeine extracted).

4. 190ml hot water added to 600 mL beaker. Stirred 5 min. Cooled in fridge for 4 h. Decanted 190 mL to 2nd beaker (9% of 1.6 g codeine extracted). This means that 92% of the total codeine/caffeine was extracted into a net volume of 750 mL (1.47 g codeine, 2.74 g caffeine). Residue remains in the beaker are mostly junk and aspirin.

5. Reduced volume in 2nd beaker to 150 mL by heating (use hot water but not boiling to avoid decomposition of codeine ~85-90 deg). The room fills with the mild smell of vinegar as some aspirin decomposes. The solution is cooled in the fridge and then filtered. Some amount of caffeine is filtered off at this step. Filter the solution using whatever you have. Coffee filters work well, but lab filters work the best. Just make sure you don't end up with obvious solids in the filtered solution. This will take about 1 hr. You may also want to rinse the solids left over in the filter with minimal ice-water to extract any remaining codeine. What you're doing is actually
recrystallizing the caffeine, and for people who haven't seen it before, it almost looks like cotton candy.
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Dried codeine product from a cold water extraction on a pyrex tray.
6. Then the volume is again reduced to 50 mL. The solution is cooled in the fridge and then filtered. More caffeine is filtered off at this step. After this treatment, less than 15% of the original amount of caffeine will remain in the solution.

What remains is a solution of codeine without a discernible amount of caffeine that leaves a truly euphoric stoning codeine. The solution can be evaporated down to a powder that looks something like brown sugar and is intensely bitter (unlike caffeine, that is only mildly bitter). This is a relatively concentrated form of codeine phosphate that you're after. Note how this technique also does not use any acids, bases or organic solvents to accomplish the removal of caffeine from the caffeine/codeine, and thus I feel is a significant breakthrough.
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Final scraped and dried aspirin product from a cold water extraction. This final extraction should theoretically only contain codeine and pill binders, with negligible amounts of ibuprofen remaining.

Video manual of Cold Water Extraction

Solubility of ibuprofen and paracetamol

These figures should be taken as approximates only. Don't forget, this only includes how much para/ibu is dissolved, and does not include suspended solid particles of paracetamol and ibuprofen. The purpose of filtering is to remove as many of these solid particles as possible. If filtering is not done properly, toxic levels of paracetamol or ibuprofen can remain in your final product.

Solubility of Ibuprofen
The solubility of ibuprofen in water at 25 degrees Celcius or lower is less is than 1 mg per mL.
At 31 ºC, 100 mg dissolves in 100 ml (1 mg/mL).
At 21 ºC, 7.8 mg dissolves in 100ml (0.078 mg/mL)

Solubility of Paracetamol
Mg paracetamol dissolved in mL of water at degrees Celcius.
0 ºC — 7.21 mg/mL
5 ºC — 8.21 mg/mL
10 ºC — 9.44 mg/mL
15 ºC — 10.97 mg/mL
20 ºC — 12.78 mg/mL
25 ºC — 14.90 mg/mL

FAQ

Can every combo med be Cold Water Extraction?
No. Some combo meds also contain a third ingredient, such as an anti-cholinergic. If this third ingredient is potentially dangerous and soluble in water, a Cold Water Extraction will not remove that risk.

Can the solution be evaporated to be used for other purposes?
Yes, although the solution is going to contain some binders, fillers and some amount of the combo med we didn’t want. Hence, depending on the drug, the powder could be used for snorting, eating later or plugging, but would in no way be ideal for IV (intravenous) use (
POTENTIALLY FATAL - DO NOT ATTEMPT THIS). Most drugs that come in combo-med form are, as far as I know, not suited for smoking. To find out whether the drug you have separated can be used via a certain method of administration, use the search engine or ask here.
 
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master009

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استخراج آب سرد روشی است که برای جداسازی ترکیباتی که با استفاده از t با هم مخلوط می شوند استفاده می شود
G.PattonPlease tell the solubility of codeine
 

G.Patton

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Please tell the solubility of codeine
master009Soluble in ethyl ether, benzene, chloroform, toluene; very soluble in ethanol; insoluble in petroleum ether; Slightly soluble in cold water and well soluble in hot water
 
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master009

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Soluble in ethyl ether, benzene, chloroform, toluene; very soluble in ethanol; insoluble in petroleum ether; Slightly soluble in cold water and well soluble in hot water
G.PattonThanks . please tell Solubility table of codeine in water
 

master009

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Can you clarify your request please? Are you looking for codeine phosphate or free base? It is important.
G.PattonI mean codeine pills .codeine phsphate or hcl or sulfate.
I searched and came up with these numbers.
100mg/ml (61 F)
33mg/ml (0 F)
Are these numbers correct?
 

G.Patton

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I mean codeine pills .codeine phsphate or hcl or sulfate.
I searched and came up with these numbers.
100mg/ml (61 F)
33mg/ml (0 F)
Are these numbers correct?
master009codeine phosphate's water solubility is 1 g in 2.5 mL and codeine sulfate's water solubility is 1 g in 30 mL

Its salts very soluble in water
 

jit123321

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Sir how to synthesis tramadol crystal from tramdol hydrochloride tablet 100 mg sr
 

prind

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Can you extract codeine from syrups too? (whit a Cold Water Extraction)
 
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