Author Topic: first experiment in throwing eudragit a success  (Read 4462 times)

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barkingburro

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first experiment in throwing eudragit a success
« on: June 25, 2004, 01:51:00 PM »
swibbs had this funny notion for some time that the best way to solve out extraction problem is to mimic mother nature. here's the first experiment and its results :

48 60mg white gweneric 'suphedrines' with Chlor, MCC, and Magnesium Stearate. (these pills had been previously un gaaked, but it seems of recently have found them selves gaaked with presumably eudragit)

1> 48 pills were placed un ground into a beaker.
2> to beaker was added 400 ml of d/h2o
3> hcl (34%) was added (approx 5 ml) drop wise until ph was brought to 2
4> beaker was placed over med heat and brought to appox 100 deg F while stirring moderatly. (pills begin to break apart on own)
5> beaker was left on heat at 100 deg F for 20 minutes with occasional stiring. (pills will have pretty much fallen apart by now)
6> to solution was added a 35% NaOH solution until ph was brought to 6-7.
7> solution was kept at steady 100 deg F heat and stirred occasionally for an additional 20 minutes.
8> an additional amount of 35% NaOH solute was added until ph reached 12. 75 ml of fresh xylene was added to solute.
9> temp was raised and 10g of NaOH was added to solution when temp reached 160degF. (this rxn was rather violent) and solution was allowed to reach near boiling temps and remained there for 20 minutes. at this point two noticble things occured. the solution started turning coffee brown (similar to festers description of using KOH) and a gooey film floated to the top.
10> after 20 minutes the solution was removed and seperated via sep funnel. about 50 ml of coffee colored solute was left in bottom of sep with goo and np on top. to this was added approx 15g of rock salt. enough rock salt was used to completey fill the 50 ml of coffee fluid in sep funnel.
11> sep funnel was slowly drained until almost all of the coffee fluid was out of sep and back into beaker with rest of 'coffee'. to this coffee and additional 75ml of xylene was added, placed on heat and once again brought to a near boil for 20 minutes.
12> NP and goo left in sep was now filtered through rock salt in the sep. NP came out goo free and rather clean. sep was rinsed with a samll amount of d/h2o and the NP and water mix was set aside and covered.
13> coffee was removed from heat and allowed to sit over night. next day the same rock salt in sep funnel procedure was repeated.
14> all NPs were combined and rinsed 1 time with d/h2o.
15> 2 pulls of aqueois hcl were used to extract pfed from NP. after evap initial yield is approx 1.4g of 2.88g available.

intially the yield is rather disappointing, but swibb has ideas as to where the p/fed may have gone. the product however is pristine. next swibb plans to try this on other mixes of pills, and make a few mods, such as less water and gassing instead of using aqueos hcl. as a summary here's the basics : mix uncrushed pills and h2o, acidify to 2, heat to 100degF for 20, then raise ph to 6-7 remain heated for 20, raise ph to 12ish and heat to 160, ad NP, add NaOH,
and bring to near boil, leave on heat for 20 more, decant non polars, wash and then drop out your p/fed.

will update with next experiment

ChemoSabe

  • Guest
Approximate Yeilds & Reaction Test?
« Reply #1 on: June 25, 2004, 02:43:00 PM »
Even if you feel you can improve the yeild it's still a good idea to report it.

I won't pass judgement and it's helpful to know to get a gauging and estimation of what might bee going on in the process.

Plus a reaction test is the real proof of your pudding. Especially concerning the rather funked up results which can often occur from these newer breeds of pill gakks.

But congrats on what you've done so far and looking forward to more results and further progress.

PS. I like the variation on your name "barking burrito".  8)


geezmeister

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missing pseudo
« Reply #2 on: June 25, 2004, 05:28:00 PM »
I suspect your yield loss is vaporized freebase pseudo that escaped with evaporating nonpolar solvent as you boiled the polar layer. Do the boils in a flask and direct any vapor through a condenser set up for distillation and you won't have the loss. My guess.

Excellent procedure derived from studying recent posts by former_Chemist and fester. I look forward to reports of how the pseudo so obtained reacts.

The process seems susceptible of scaling up and this offers a benefit over Prepuce's short path distillation method, which I think will be more difficult to scale up.


Prepuce

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Another data point
« Reply #3 on: June 25, 2004, 11:02:00 PM »
SWIP had a small amount of the dreaded yellow oil left as a result of a failed experiement, so he tried to put it to good use. It was noted at the outset that the oil contained many tiny, white particles suspended in it.

Test One:
2-3 drops of the the oil were placed in approximately 5ml dH2O. The oil floated on top. Approx. 1 ml strong NaOH solution was added. The oil lost it's yellow color, and at once white particles began to precipitate, then hung in suspension in the NaOH/dH2O solution.

Test 2:
A few drops of the oil were mixed with several drops of ammonium hydroxide solution. A white precipitate formed and became suspended in the ammonia water, but the yellow oil remained floating on top.

Test 3:
1 drop yellow oil was combined with 1-2 ml of xylene. The yellow oil fell to the bottom, but did not combine. The tiny suspended particles did combine, entering into solution with the xylene. Addition of approximately 1ml ammonium hydroxide had no effect on the oil, but caused the precipitation of a white substance from the xylene. SWIP believes the precipitate to be pfed freebase.

Conclusion: If you wanted to recover the pfed from the xylene after basing with NaOH you would have a hard time, because the gak keeps it in solution. Ammonium hydroxide, on the other hand, appears to base the Pfed but not the gak. Other bases would probably work similarly.

SWIP has noticed in his gakinator experients that as soon as he used HaOH the game was over. At times he wondered if he couldn't pull the pfed more quickly if he combined the ammonia with a few mls of NaOH. He found that once the NaOH was in he could add all the ammonia he wanted, but the pfed wasn't coming out.

Geez:
"The process seems susceptible of scaling up and this offers a benefit over Prepuce's short path distillation method, which I think will be more difficult to scale up"

You may be right, but the more SWIP uses the method the better he likes it. Once the setup is put together, (and SWIP doesn't take it apart), you just dump in the freebase, put in the ice, and heat. Set it and forget it!

In fact SWIP doesn't recommend forgetting it, but he was been guilty of doing just that for nearly an hour. When he came back the beaker was stuffed full of delicate, shimmering crystals. No harm had been done, it just sat there recylcing itself until he returned.

SWIP believes that it would be difficult to outdo the purity that is easily achievable with this technique, and the only difficulty he would anticipate in scaling it up is the fact that he would need a larger beaker and test tube. The gakinator extraction procedure isn't mature yet, however.

PP

UncleFester

  • Guest
the missing product...
« Reply #4 on: June 26, 2004, 12:08:00 AM »
I like that two phase protective system you thought up. It's pretty slick, and I would have thought that the eudragit would have went there and sought refuge from the NaOH. It must be that once it gets knicked on the sides, its solubility changes and gets whacked. As to your loss of product, if pseudo was so easily volatilized, then steaming it out the the gak pills would be a breeze. What I believe you are seeing is the old "psuedo burn" where unseparated pills ingredients can react with NaOH and the pseudo and make a regrettable mess. My bet is that's where it is.

barkingburro

  • Guest
yield was approx 50%
« Reply #5 on: June 26, 2004, 12:17:00 AM »
yield was approx 50%, 1.4 of 2.88g avail.

geez swibb will try with the addition of condensor, dunno why swibb didn't think of that before hand. swibb will be attempting a much larger batch soon, as well as a mini experiment with 120's.

PP : one of the differences i think in your experiments and mine are a> the times involved and b> the ph levels.

the way the eudragit works is basically like this (so far as i have been able to discern) : there are multiple parts to the delivery system the first part is designed to wear away the intial encapsulation in the stomach at a ph of approx 2. this takes about 15 - 20 minutes. the psuedo is intended to then be released in the duodenum where the ph is 6.2 - 7. (in further research swibb found that the body actually raises the ph at this point using sodium bicarbonate (baking soda) so swibb plans to use this to accomplish the initial ph rise.) the doudenum is where the majority of the drug is released as the remaining portion of eudragit (and other similar hydrogels) absorbs water and expands becoming porous enough to release the drug. the remainder of the drug is released over a 2 hour period as it passes through the digestive system.

IMHO time is a very important factor in the release of the drug in this manner. perhaps KOH is going to be the best thing to use, but swibb is going to modify a few times and get back with the results.

UncleFester

  • Guest
KOH
« Reply #6 on: June 26, 2004, 12:49:00 AM »
I'll repeat this on my thread, but when you evaporate down the alky, be sure to bring it to a boil at least once, as more crap comes out after the main load, and for the brand name pills, it would be best to bump up the KOH to 10 grams per 100 pills. They have more goo in their expensive pills.

UncleFester

  • Guest
how do I spot polymer??
« Reply #7 on: June 26, 2004, 02:52:00 AM »
If you shake with solvent with the water phase and get milkshake, you either have polymer or detergent...detergent is easy to get rid of...
If you shake with solvent, and there is a bunch of crap between the water layer and the solvent layer...you may have dragged in shit, but the bet is detergent...
If you shake with solvent, and the solvent won't clear...that is polymer...
No clear face between the water and solvent.... that is polymer... or detergent...
To get a clean product one must pay attention to these deatails.
A good clean up will have a sharp dividing layer between the solvent and the water layer

geezmeister

  • Guest
don't be discouraged by the yields
« Reply #8 on: June 26, 2004, 03:04:00 AM »
Don't be discouraged by the yields. Yields from a/b extractions of pills are usually less than other methods, but also are generally cleaner. I always found a "wall" around the 60% mark on a/b extractions. Every method I used, when I got it ironed out, seemed to hit a wall at 60% yields. Th waterless a/b started out at 40% and I played with it until I could get a sixty percent yield. With Straight to B we hit the same wall. When we went past it, we fooled ourselves. The extra weight was PEG. My point is that there is probably about ten percent improvement in overall yield to grab before that wall is there again, and frankly, that may be a good tradeoff point between yield and purity.

I had little success steam distilling pseudo in the past. When I was cleaning freebase pseudo crystals and did it in hot water, and particularly in boiling water, the room filled with the sweet aroma of freebase pseudo, and my yield went way down. I've also left a ker plunck for pseudo run too long and evaporated a lot of naptha off and had poor yields. I don't think steam distillation and losses of the sort I am talking about have the same things in common. Its one place too look for missing yield.


ChemoSabe

  • Guest
Yes, That's Success
« Reply #9 on: June 26, 2004, 11:04:00 AM »
barking Burro wrote...

yield was approx 50%, 1.4 of 2.88g avail.

That's extraction success in my book. Particularly concerning the isidiousness of this newest king of the gakks.

A reaction of the extract is now in order with a following bioassayed celebration.

Wishing you luck for proving this pudding.


gluecifer69

  • Guest
Great Work BB
« Reply #10 on: June 26, 2004, 03:54:00 PM »
Swim is going to give this a go on some 120's and report back to thread later in the eve.

Good job!

Now we have three different cures for our new gakk(gakinator,Fester's and BB's), things are looking better all the time.


abominator

  • Guest
an extraction w/ BB's method
« Reply #11 on: July 12, 2004, 02:06:00 PM »
will be done tonight, since no bee has posted any yeilds from reactions or even the extraction besides BB.  The feedstock will of course bee flushed down the toilet to react in the septic system.


barkingburro

  • Guest
new info and a slight modification wanna hear it?
« Reply #12 on: July 12, 2004, 03:02:00 PM »
ok friends, this batle has been a fucking bugger but i think we have a way to beat its as down WITH HIGH YIELDS.
if following this thread please refer to the newest one i am going to post but along the lines of this thread some good news :

swibb has reacted the psuedo from this method and came out mighty fine. yield was about 50% on the h3po3 burn which is low ion swibbs books BUT that is largely the fault of not having the temp high enough.

swibb has no with a slightly modified method gotten 25-35% yileds of clean P/fed from 120's and a very very high yield gaak free from 60's. news to come.

cycosyince

  • Guest
is it w or w/o
« Reply #13 on: July 13, 2004, 11:25:00 PM »
Are all the pill batches known to have a gakk problem prior to extract? Rather should I ask, are ungakked pills in your area a memory?
The extract looks simple enough... `,) 8)