Author Topic: Strange pill extraction.  (Read 2661 times)

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meths

  • Guest
Strange pill extraction.
« on: August 28, 2004, 05:44:00 PM »
Hello all,

Swim needs some help with a funny pill extraction result. Here is what he did:

1. Ground 3 packets of 120mg Sudo Sulfate pills in a mortar and pestle. These pills also contained Loratadine and Chlorpheniramine maleate.


2. Soaked the pill mass in MEK overnight, filtered and dried the PM.

3. Added xylene, soaked overnight.

4. Boiled xylene/PM mixture, solution turned yellow. Swim thinks this is from the sugar that was coating the pills melting (He obviously should have removed this first. Pill mass became a single solid mass. Swim thinks the sugar melted and fused all the powder together.

5. oops, wrong number! go to 6.

6. Xylene was poured off, more added and this also decanted off.

7. Mineral turps was added, boiled for 10 min and decanted.

8. Dry acetone was added, boiled for 10-15 min and decanted.

9. Pill mass was washed several times with more acetone.

10. At this point, swim realised that no NP solvent was going to dissolve the burnt sugar, so he added dilute HCl solution and xylene and left overnight, hoping the HCl would break up the PM, and the xylene would clean the solution.

11. Swim removed some of the HCl solution, based it with NaOH, and added mineral turps (ran out  of xylene, and had no other NPs lying around).

12. After shaking and giving time to settle, mineral turps was decanted off and washed 10x with NaOH solution.

13. a few ml of HCL were added, shaken, and separated from the turps with sep funnel.

14. The HCl soln was a bright yellow colour, so xylene was added, hoping this would clean it. It did not.

15. The HCL/xylene mixture was dumped into a watch glass and evaporated.

16. At near complete evaporation, acetone was added, and beautiful white fluffy crystals appeared, in quantities "that seemed about right" much to swim's delight.

17. Now for the problem. Swim doesn't think this white powder is pseudo. It don't taste great, but not really so offensive you have to spit it out like sudo.

Anyone have any idea what this stuff is?? Swim was thinking it might be one of the antihistamines, but there is just too much of it (the pills only have a few mg of antihistamines). Going by taste, swim would think there is almost no sudo at all. Any ideas? Did he burn the sudo when boiling?? What is going on? The powder is a beautiful clean white. The NP was washed very very well with naoh solution before adding hcl. The powder is not particularly bitter and does not burn the tongue or anything. Help please.

Cheers.

psilly1

  • Guest
Does it taste salty?
« Reply #1 on: August 28, 2004, 06:22:00 PM »
May be salt from the HCL/NaOH neutralization. How high did you get your temps when doihg your boils?

meths

  • Guest
No, it doesn't taste salty.
« Reply #2 on: August 29, 2004, 09:29:00 AM »
No, it doesn't taste salty. A really hard taste to describe actually. Does taste "organic" though. How could there be salt when I washed the NP so many times??

Cheers.

SQUIDIPPY

  • Guest
burn test
« Reply #3 on: August 29, 2004, 10:24:00 AM »
Burn Test 101

1.) Place small amount of subtance in question, on small piece of aluminum foil.

2.) Apply heat to the underside of foil, (a lighter works well)

3.) Apply heat until substance has burned away.

4.) Observe residuals left on foil. {Hint : Pure p-fed will only leave a dark "stain" on the foil)


Rasputin

  • Guest
Strange Pill Extraction Indeed
« Reply #4 on: August 29, 2004, 10:53:00 AM »
Hello:
First of all there could be salt because, unless you wash with some plain DH2O last there will always be some sort of leftover sodium ions, these will make salt upon acidiffication. With P-Fed taste is really not a good thing to go on, many things in the pills, including the antihistamines, have that very bitter/nasty/sour taste. Unless you have been cooking alot, taste wont be of much help.

As far as your pill extraction goes, on the whole it was done very strangely(weird choice of solvent, and weird order of washings). I belive I know the brand of pill you used, and to remove all the shit well, the soaks and boils need to be done in a certain order. If the pills you have are the name-brand version(with Povidone), you should have used your Turps for the soak, not MEK. If they where the generic version(no Povidone), Xylene should have been used. After your soak you should have done a Acetone(or MEK) boil or two to remove the rest of the Povidone(Povidone gets nasty at temps of 104C and up). You can still do your boils if theres a sugar coating on the pills, you just cant use Xylene with its ultra high BP, Toluene,Naptha,and Mineral Spirits are usually allright, and it does not have to be boiling, usually pretty hot is ok. The yellow color you described was most likely PEG, those pills are packed with it. When you say you removed the HCL, I hope you mean you boiled it off and not decanted because, that will certainly cost you some yield. I read your other post about using the Tetra Trap, why did you change your mind to this instead? The TT would have been much better for you probabaly, it quite user friendly.

Now as far as testing the "white fluffy stuff", you could just eat some of it. Nothing in the pills is deadly or dangerous, eating a small amount would let you now what you got, speedy=P-Fed,Sleepy=Antihistamines, nothing=Binders/Fillers. I will probably get shit for suggesting that but, it is an easy way. It only takes the tiniest amount of antihistamines to feel an effect, usually twice the amount of the boxes recommended dose so, start with a ultra tiny amount.

Oh yeah, if it turns out you did in fact fail, just remember its not the end of the world and, we all failed our first times(three times for me). So stick with it and keep learning and trying, anyone can be good at this, it(like all things) just takes time,practice, and above all else the desire to never stop learning.

Good luck fellow Bee, may you always be prosperous.


meths

  • Guest
Rasputin:
« Reply #5 on: August 29, 2004, 11:21:00 AM »
1. OK, I will wash with Dh20 next time. Oops, really messed up there.

2. I mentioned the taste part because there was NO bitter taste at all. I would have thought that even the slightest
bit of pseudo would be obvious.

3. I intended to switch to the TT after the boils, but when the mass went solid, I thought I really had to use a water based method to dissolve it OK. I thought the molten sugar might lock up the pseudo.

4. I did in fact eat the stuff, but can't say I really noticed any effect.

OK then, my next move is to do the TT, and stick to the rules. Does this technique still work OK with the modern gakks? Seems some people are relying on Japan Drier soaks. What about fester's KOH/ISO method??

Thanks for your advice.

Rasputin

  • Guest
Pill Extraction Stuff
« Reply #6 on: August 29, 2004, 03:07:00 PM »
All of the current pill extractions work, as long as you dont have Eudragit in your pills. As it stands there is no real way to test for it, you just have to assume it there and proceed acordingly. UncleFester's ISO/KOH works on Eudragit tainted pills, I have used it with sucsess, and so have many others. I only mentioned the TT because it seemed like you had your heart set on it and, its often hard to change peoples minds. Besides contrary to popular belief, not all pills out there have Eudragit in them, just most of them. Lately I have been finding a certain brand that doesent have it in them so, for the time being the old ways are alive and well for me. Anyways, use the ISO/KOH extraction its really easy, only annoyance is the KOH(I ended up just ordering some from a chem supply, it was cheap and easy).

P.S. If there was no bitter taste at all, not even the slightest, you probably dont got it, its usually quite vile tasting.

Good luck Bee.


Shane_Warne

  • Guest
TT will work to some extent on most (All?
« Reply #7 on: August 30, 2004, 04:48:00 AM »
TT will work to some extent on most (All?) pills.

It's orange susceptable if heating-especially strong heating's used.

It's got no denfense against yellow either, and this will show up whether heating is used or not.

Try 2 dry MEK/JD boils, 2 50/50 xylene/naptha boils-->Dry completely-->4hr TT with stirring

Untested, take it for what it's worth. Nothing much can go wrong.

UTFSE for eudragit too.