Help - Pill extraction issue

[kris_1108]

Swik is stuck half way in an extraction of 192 30mg pills (total 5.76gms avail)

Each tablet contains the active ingredients Ibuprofen BP 200mg and Pseudoephedrine Hydrochloride PhEur 30mg.
Also contains: Calcium Phosphate, Microcrystalline Cellulose, Polyvinyl Pyrrolidone, Sodium Carboxymethyl Cellulose, Magnesium Stearate, Hydroxypropylmethyl Cellulose, Talc, Titanium Dioxide, Quinoline Yellow and Sunset Yellow (contains Aluminium), Shellac, Block Iron Oxide.
The pills have a yellow but not glossy coating.

*Ground the pills in a coffee grinder. ~120gms of powder including 38gms of ibuprofen (soluble in xylene and acetone)

*The PM came up to the 100mL mark in the beaker. Added xylene to the beaker to the 300mL mark. Boiled, went BRIGHT yellow. Decanted as much as possible. Left with a slurry of xylene/PM. Repeated this 3 times, on the last time, the YELLOW PM/xylene was poured through a filter and wrung out and returned to the beaker.

*Added acetone to the 300mL mark. Boiled in acetone, decanted yellow acetone through a filter, wrung out, returned to beaker.

*Added 250mLs of 96% ethanol to extract pseudo.

The alcohol is CLOUDY and YELLOW and will not filter. A tight packed charmin dripping once every 10secs will not clear the alky.

Now what?
Swik is thinking, evap the alky from the PM. Proceed with something else.

Ware? Geez? Any of the other Superbees?

[ChemoSabe]

That's what I'm on the verge of.

Then I think it's gonna bee homebrewed e or nothin'.

Pills suck and fermentation is the future.

[kris_1108]

Thanks Chemo but that does not help me with my existing problem.

I have a beaker with 3/4inch of yellow Ground Up Pills and about 250mLs of yellow alcohol that wont filter.

I REALLY DONT want to have to a/b, but I may not have a choice.
I might have to evap the alky/dry the PM. And then add 6mgs of sodium carbonate, 100mLs of xylene, and 15mls of ethanol. Filter off and boil the YELLOW NP till 105°c. Wash with NaOH, hot water, cool water. Then titrate and HOPE BIG BIRD DOESN'T FOLLOW ME! (the yellow shit.)

The PM does NOT cloud up xylene or acetone. It does, however, cloud up alcohol.

I would really appreciate some input from knowledgeable bees on this.

Thanks

[Osmium]

Try cold, diluted HCl.

[unionpacific]

I would put everything back in the flask including the tissue plug, add a bunch of more dry etoh warm the flask up a little bit and set the flask at an angle so all the PM and tissue is at one side and decant as best as you can, repeat it 3 times, filter the last of the decant or any etoh that has chunks in it, gravity filtration really sucks when dealing with this type of mixture. vacuum filtration flask and a good adjustable vacuum will make it a breeze, also clean sand can be used to filter such mixtures.

If you evap the etoh and you see no pinwheels and it starts burning there was gaaks in,I doubt it's gonna happen but it might. But at least you got rid of all the PM and have rough dirty ephedrine to clean up assuming your evap dish is full of pinwheels ready to be scraped with a brand new razor

BTW those pills have alot of shit in them and not much ephedrine, But it's all just experimenting right??

[lsd]

I too had a similar problem except I left the yellow behind.
After basifying, an emulsion from hell existed that couldn't be broken. To fix this, the emulsion was then scooped out (leaving the yellow(orange)behind), steam distilled (in small portions), neutralised with hydrochloric acid and evapourated. Dissolved in small amount of ethanol and evapourated once more, leaving lovely pinwheels that we all want. It worked but don't know the losses, etc. More investigation is needed and as these sort of pills are my only source, investigate I will!

[kris_1108]

Thanks guys for the help.

I will go with unionpacifics idea and decant the EtOH, and repeat the add/decant (to get all the pseudo.)
And then evap for dirty p-fed. Will then proceed with more washes.

Will keep ye posted.

Os, what will the HCl do? Will is destroy the stuff that is clouding up the alcohol? Or will it encourage it to settle out?

[Osmium]

> Will is destroy the stuff that is clouding up the alcohol? Or
> will it encourage it to settle out?

It will make some of the stuff precipitate out.
BTW, I hope you do not work with all your pill mass. Whatever you do, test it with a small amount first. No need to send it all down a one way street.

[ordinaryguy]

in swio's experience a/b's offer the highest yield and cleanest product when sequenced correctly. the key is to do DH2O washes prior to gassing or titriating and after the bulk of the non-essential ingredients have been filtered off. of course don't forget do dry you NP prior to gassing. if you would like more info let me know and swio will send you her favorite extraction tech. it doesn't involve alchohols or multi-solvent washes. it rely's a little on the taste buds wihich don't lie if you know what i mean. also being that you are from down under i'm not sure if the store chain is located there but where swio comes from there is a store chain that has plastic bags with big red bullseyes on them(the company logo) and they carry generic 60mg ephedrine hcl tabs with a 2mg antihistimine that work great in a/b extractions

[12cheman12]

yes we have the company with the big red bulls eye, But in australia we dont have Ephedrine/Pseudoephedrine generic brands, any products containing pseudoephedrine must be sold from a chemist and we only have the brand names. And there arnt any products you can buy that contain Ephedrine, its all pseudoephedrine.

[ordinaryguy]

All apologies! Didn't mean to rub salt in a open wound. There are also conveience stores here with gas and smokes and stuff that sell a pill with pseudo that seems to be really easy to work with. They usually sit on the check out counter and are limited to two bottles per day. They yield 2.some odd grams per bottle of 120 but are very little pills and extract via a/b nicely.

[Ewok_Poacher]

swiep had a simialr problem and he did this -- 3 acetone washes followed with 3 cold h20 pulls
H2O must be cold - mix h20 and pill sludge (or whatever) put in fridge for 20 minutes and decant the h20 - evaporate
after utfe swiep found alot of the new gacks are not soluble in cold water. give it a try , it cant hurt.

[Shane_Warne]

imho you should base it at some point and evaporate to get the fb, or gas and/or titrate.

You've done a xylene boil and an acetone boil so if you use a mild NP like petrol. ether then it isn't likely to pull all that much except pfed.

using a cotton ball in your filter helps stop blockages like that...so does super slow decanting, allowing time to settle and suitable dilution.

goodluck, I'm sure you'll be back to brag about your heroic recovery.