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Two procedures to extract from pills for which a cold water extraction would not
be enough:
IDEA Method
E-Gull Method
"Smack~M~BackDown 2003"
The Write Way
The Original E-Gull Method
For use with Non-Dry Matrix Formulations (NDMF)
The IDEA Method
For use with Dry Matrix Formulations (DMF)
Disclaimer: Introduced for informational and educational purposes only.
All abbreviations will be highlighted in RED and some will be linked to the defi
nition
Special considerations will be highlighted in BOLD
The main purpose of these two methods are to effectively isolate polymer inactiv
es and some antihistamines included in over-the-counter (OTC) medicines containi
ng pseudo-ephedrine hydrochloride (p-fed.hcl.) allowing easier separation/extrac
tion of the main excipient using alcohol (alky) as the extraction medium.
The degree of purity will vary depending on the the alcohols used, verses the fo
rmulation of OTC where either technique is applied.
Special Importance: Four major problem areas in the past have surrounded the rem
oval of Triprolidine (TRIP), Chlorpheniramine Maleate (CHLORPHEN MAL), Povidone
(POV), and Polyethylene Glycol (PEG). All four have been successfully eliminated
when a Tetrachloroethylene (TCE) Wash {E-Gull Method} was performed prior to th
e alcohol extraction stage.
To date, there exist two major groupings in formula preparations of these OTC's,
comprised of inactive ingredients (Gaak), in all strengths/brands, and are incl
uded as preferred embodiment denaturants by the Pharmaceutical Industry, identif
ied as follows:
NDMF DMF
FILTRATION
Two areas of consideration involve the filtering of the pill mass (PM) at two st
ages during this process:
Loose Filtration is to be used immediately following the TCE wash of the PM and can
be accomplished using one single coffee filter. This loose filtration is necess
ary to allow for the polys transport away from the PM via the TCE. If this flow
is restrictive, the Poly's will re-cleave to the p-fed. It's important that all
polys be removed from the PM, so this single filter/PM ball need to be squeezed
of excess TCE.
Fine Filtration is to be used immediately following the alky soaks of the PM and ca
n be accomplished using a funnel with the stem packed with either a Charmin Plug
or cotton balls and the basket of the funnel lined with 3 coffee filters. After
the PM settles in 3 times the amount of alky, the alky will be somewhat clear,
and this alky will need to be pulled off the PM, put through the fine filtration
device and collected in an evap dish.
MnkyBoy's Cracked Pearls (Tomb-stones)
If one was to come across several 120 mg/12 hr decongestants (aka Pearls), a sim
ple task to crack the shells to get at the pearls inside is to use acetone.
With the pills freshly removed from their vacuum-packed slumber place into a WIR
E MESH food strainer. (Use a strainer that isn't to fine, nor to coarse)
Place the strainer inside a bowl deep enough so that the pearls are below the to
p of the bowl
Take DRY acetone and proceed to pour enough over the pearls so that they are cov
ered with an excess of about 1/2 inch tone
After a minute or so one will notice that the pearl shells are split open and th
e pearl meat is starting to fall out. Now raise and lower the strainer in the to
ne. The pearl meat should be falling through the strainer to the bottom of the b
owl.
After a few dunks, start sifting the shells in the strainer LIGHTLY. Do not pres
s or force the hulls through the strainer.
Discard the spent hulls.
Decant the tone which is a milky/whitish color and add a bit more tone, enough t
o cover the pearl meat. Swirl around for a bit and then decant the tone.
Tap the bowl on the counter to dislodge excess tone and decant this tone.
DO THE FOLLOWING EXACTLY AS STATED FOR OPTIMAL EFFECTIVENESS: Set the tone wette
d pearl meat aside with a fan lightly blowing ACROSS the top of the bowl or at a
slight angle.
WALK AWAY
After about a half hour check the contents of the bowl. Notice a top skin layer?
Is it cracking? Carefully check the underlying powder to see if it is still sat
urated with tone. If so let it dry longer. If it is dry, carefully remove the pl
astic skin layer from the top of the powder. Discard. (Or use it at the park nex
t time as a frizbee). If after extracting the e from the PM, yields are low, che
ck the skin you pealed off. If the tone was wet, this skin can contain some e. H
int: That's why the DRY tone.
Do with the fine powder as one wishes.
Ingredients for The E-gull Method
1 box NDMF p-fed (any count...24,48,96)
1 can TCE
Denatured Alcohol
Ingredients for The IDEA Method
1 box DMF p-fed (any count...24,48,96)
1 can TCE
Denatured Alcohol
Isopropyl Alcohol
Acetone
Utensils Needed For Both Methods
Mortar&Pestle
Fine Strainer
Evap Plates
Funnel
Single edge Razor Blade
Coffee Filters
Cotton Balls
Tall Glass Jar (Spice Jars work well)
Stainless Steel Bowl
Pipette, eyedropper or syringe
Non-Descript Items of Importance for NDMF & DMF
If Using RedHots (pills with red dye coating), it is important to visually identify
the type coating used. There are two types to date. One consists of a shiny coa
ting and the other a dull coating. The shiny coating can be rinsed off without b
reaking into pill. This is done by soaking for a few minutes in a small amount o
f acetone (tone) followed by rinsing the pills with distilled water (dh2o) until
the color washes off. This can be done in a large strainer or colander. It's im
portant to put these washed pills onto a paper towel and allowed to dry before c
rushing, especially if the DMF is present. The skin barrier between the pill and
the coating will be somewhat sticky when damp and it's possible to remove that
skin by gently rubbing the pills between the paper towels thereby removing one m
ore obstacle from the picture.
The dull coating presents a problem with the above procedure because the outer l
ayer consists of some of the main excipient (hence, the dullness) and washing te
nds to penetrate the pill surface causing some yield loss. It is safe to proceed
without removing the outer coating on these types.
The importance in crushing the pills to a fine powder is critical to success. The s
urface area of the p-fed must come in contact with the TCE in order to separate
and attract the polymer molecules (polys) away from the p-fed. This is especiall
y critical with the DMF pills because of the dry compaction method they employ i
n pressing these formulations.
The first phase of both these methods is a wash only....NOT A SOAK! If the pills ar
e allowed to sit in solution for longer than necessary, the polys will re-bond w
ith the p-fed and stay behind with the PM upon filtering! It's necessary to sque
eze off the excess TCE after the PM is poured into the single filter following t
he TCE wash. If poly re-bonding occurs, a re-wash will become necessary after co
mpletely drying the PM. Drying can be achieved by simply pouring the PM ball ont
o a Legull size sheet of notebook paper, breaking up and spreading out. Drying c
an be sped up by moving this gritty PM powder around on the sheet of paper and g
rease spots can be seen where ever the damp PM has been! Complete Dryness is ach
ieved when the Dry Cleaner smell is no longer present.
After the TCE wash and dry, you're ready to proceed into the second phase or the ex
traction phase. This phase, it has been learned, is time sensitive as well. Any
shortcuts or deviations will result in unexpected results, lower yields, or GAAK
being pulled along with the p-fed. The Dry PM should be put through a fine siev
e strainer, collected onto a piece of paper and then poured into a tall jar capa
ble of holding the PM plus 75% more in liquid volume...i.e. PM=25% Alky=75%.
The Alky needs to be poured onto the PM inside the jar, then stirred well. This
extraction solution needs to settle until the alky is clear. The alky needs to b
e pulled off the top of the PM, without disturbing or collecting any of the PM.
Then this liquid needs to be put into a fine filtration device and collected ont
o an evap plate. Repeat this addition of alky to the PM until all p-fed is pulle
d from the PM. DO NOT HEAT this solution to speed up drying. Up to 50% yield los
s has been reported when heating was performed by others and the only explanatio
n for this would likely be due to evaporation. The evap plate can be put on top
of a lampshade that puts at least 6 inches or 15.24cm between the bulb and plate
.
NOTE...If using redhots and they are shiny, remove and dry prior to crushing
Step2
Measure out Tetrachloroethylene (TCE) to ~3 times the volume of Pill Mass (PM) i
n separate tall jar.
Step3
Put crushed PM in SS Bowl and pour the TCE over the PM. Stir until all floats fr
eely in solution and immediately pour all into Single Coffee Filter lined funnel
with no stem packing. Take can of TCE with Spray Tube provided and spray down s
ides of filter to collect all PM in the bottom of filter. Carefully squeeze exce
ss fluid out of filter and PM to remove as many polymers as possible.
Step4
Open Filter and pour the PM ball onto a piece of Legal Sized Printer Paper. Brea
k up PM ball and spread out flat to dry. Dry thoroughly at room temp until no dr
y cleaner smell is detected. Do Not Heat! Moving PM around on paper assists in d
rying. When dry, pass gritty PM through fine sieve strainer. Pour PM powder into
clean Tall Glass Jar.
Step5
Cover PM in jar with denatured alcohol (alky) to ~3 times the volume of PM. Stir
thoroughly and let settle until the alky is clear. Settling time will vary depe
nding on amount and type of inactives (Gaak) initially present. Never let this P
M sit too long past the clear stage because it will start to absorb the Gaak.
Step6
While waiting, set up fine filtration device. Either Charmin plugged funnel or c
otton ball packed stem/multi-layer coffee filter lined basket funnel.
When the alky/p-fed solution is clear, pull the alky off the top of the PM witho
ut disturbing or collecting any of the PM and put the solution into the fine fil
ter funnel that's positioned securely over the evap collection plate. Repeat Ste
p5 three times or until 90-95% of the expected yield is pulled and collected.
Step7
The later pulls may reveal some strange crystals in the collection plate. Prior
to scraping, a simple re-dissolve using alky and swirling will expose the pinwhe
el crystals which should collect in the center of the plate upon re-evaporation!
Scrape up just the pinwheel crystals. Save the strange crystals for a re-re-diss
olve after amassing several plates full for optimum recovery!
The IDEA Method
Step1
If using 120mg (12hr)or 240mg (24hr), An outer coating exists that would be bett
er if it's removed first. This can be accomplished by either using Mnkyboy's Ace
tone Soak or simply cracking the outer layer with a mortar and pestle and passin
g through a strainer.
Crush Dry Matrix Formulation (DMF) pseudo-ephedrine (p-fed ) pills to a powder a
nd pass through a fine sieve strainer.
NOTE...If using redhots and they are shiny, remove and dry prior to crushing
Step2
Mix as follows in separate jar: (IDEA Juice)
60%
15%
15%
10%
TCE
Denatured Alky
Isopropyl Alky
Acetone
Step3
Put crushed PM in SS Bowl and pour the IDEA Juice over the PM. Stir until all fl
oats freely in solution and immediately pour all into Single Coffee Filter lined
funnel with no stem packing. Take can of TCE with Spray Tube provided and spray
down sides of filter to collect all PM in the bottom of filter. Carefully squee
ze excess fluid out of filter and PM to remove as many polymers as possible.
Step4
Carefully open filter and pour the PM ball onto a GLASS plate. Don't use paper f
or the drying surface. Break up PM ball and spread out flat to dry. Avoid handli
ng too much while wet as the p-fed will attach to whatever it touches. Dry thoro
ughly at room temp until no dry cleaner smell is detected. Do Not Heat! When dry
, pass gritty PM through fine sieve strainer. Pour PM powder into clean Tall Gla
ss Jar.
Step5
Cover PM in jar with denatured alcohol (alky) to ~3 times the volume of PM. Stir
thoroughly and let settle at least three hours until the alky is clear. Settlin
g time will vary depending on amount and type of inactives (Gaak) initially pres
ent. Never let this PM sit too long in alky past the clear stage because it will
start to absorb the Gaak.
Step6
While waiting, set up fine filtration device. Either Charmin plugged funnel or c
otton ball packed stem/multi-layer coffee filter lined basket funnel.
When the alky/p-fed solution is clear, pull the alky off the top of the PM witho
ut disturbing or collecting any of the PM and put the solution into the fine fil
ter funnel that's positioned securely over the evap collection plate. Repeat Ste
p5 two times or until 50-70% of the expected yield is pulled and collected.
Step7
Also while waiting after filtration device is set up, pour denatured alky on top
of the reserved IDEA juice, cap and shake. Let sit until the denat separates to
the top. After all the initial p-fed is pulled off the PM and filtered, put the
denat/pfed through the filter that was collected off the top of the IDEA juice
and collect in a separate evap dish!
Step8
If any pulls reveal some strange crystals in the collection plate. Prior to scra
ping, a simple re-dissolve using alky and swirling will expose the pinwheel crys
tals which should collect in the center of the plate upon re-evaporation!
Scrape up just the pinwheel crystals. Save the strange crystals for a re-re-diss
olve after amassing several plates full for optimum recovery!
Last edited by bogumil; 07-11-2005 at 07:07 AM.
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Default Re: Extracting from pills
Glossary
Tetrachloroethylene or Perchloroethylene
Molecule derived from ethylene in which all hydrogen atoms are replaced by chlor
ine atoms; used as a degreasing solvent. It's widely used in the Dry Cleaning In
dustry as well as the Automotive Industry. It is sold OTC as Brake Parts and Ele
ctrical Parts Cleaner in aerosol cans with carbon dioxide as the propellant.
Any preparation containing these two inactives combined will indicate the presen
ce of the DMF:
HydroxyPropylMethyl Cellulose (HPMC)
Microcrystalline Cellulose (MCC)
Chlorpheniramine Maleate
Monograph Number: 2198
Title: Chlorpheniramine
CAS Registry Number: 132-22-9
CAS Name: g-(4-Chlorophenyl)-N,N-dimethyl-2-pyridinepropanamine
Additional Names: 2-[p-chloro-a-(2-dimethylaminoethyl)benzyl]pyridine; 1-(p-chlo
rophenyl)-1-(2-pyridyl)-3-dimethylaminopropane; 1-(p-chlorophenyl)-1-(2-pyridyl)
-3-N,N-dimethylpropylamine; 3-(p-chlorophenyl)-3-(2-pyridyl)-N,N-dimethylpropyla
mine; g-(4-chlorophenyl)-g-(2-pyridyl)propyldimethylamine; chlorprophenpyridamin
e; chlorphenamine
Trademarks: Haynon (R. P. Drugs)
Molecular Formula: C16H19ClN2
Molecular Weight: 274.80.
Percent Composition: C 69.93%, H 6.97%, Cl 12.90%, N 10.19%
Literature References: Synthesis: Sperber et al., US 2567245, US 2676964 (1951,
1954, both to Schering). Prepn of d-form: L. A. Walter, US 3061517 (1962 to Sche
ring). Solutions: Foley, Ilavsky, US 2766174 (1956 to Schering). Pharmacology: F
. E. Roth, W. M. Govier, J. Pharmacol. Exp. Ther. 124, 347 (1958). Toxicity data
: R. B. Smith et al., Toxicol. Appl. Pharmacol. 28, 240 (1974). Comprehensive de
scription: C. G. Eckhart, T. McCorkle, Anal. Profiles Drug Subs. 7, 43-80 (1978)
.
Properties: Oily liquid,
Boiling point: bp1.0 142
Derivative Type: Maleate
CAS Registry Number: 113-92-8
Trademarks: Allergisan (Pharmacia); Antagonate (Miles); Chlor-Trimeton (Schering
); Chlor-Tripolon (Schering); Cloropiril; C-Meton (SS Pharm); Histadur (Cooper);
Histaspan (USV); Lorphen (Geneva); Piriton (Allen & Hanburys); Pyridamal-100 (B
el-Mar); Teldrin (SK & F)
Molecular Formula: C16H19ClN2.C4H4O4
Molecular Weight: 390.87.
Percent Composition: C 61.46%, H 5.93%, Cl 9.07%, N 7.17%, O 16.37%
Properties: Crystals, mp 130-135. uv max (water): 261 nm (e 5760). Soly in mg/ml a
t 25: ethanol 330; chloroform 240; water 160; methanol 130. Slightly sol in benzen
e, ether. pH of a 2% aq soln about 5. LD50 orally in mice: 162 mg/kg (Smith).
Melting point: mp 130-135
Absorption maximum: uv max (water): 261 nm (e 5760)
Toxicity data: LD50 orally in mice: 162 mg/kg (Smith)
Derivative Type: d-Form
CAS Registry Number: 25523-97-1
Additional Names: Dexchlorpheniramine; d-chlorpheniramine
Properties: Oily liquid. [a]D25 +49.8 (c = 1 in DMF).
Optical Rotation: [a]D25 +49.8 (c = 1 in DMF)
Derivative Type: d-Form maleate
CAS Registry Number: 2438-32-6
Trademarks: Fortamine; Isomerine; Phenamin (Nycomed); Phendextro; Polamin (Scher
ing); Polaramine (Schering); Polaronil (Schering); Sensidyn (Leiras)
Properties: Crystals from ethyl acetate, mp 113-115. [a]D25 +44.3 (c = 1 in dimethyl
5. d424 1.04. nD25 1.511. Flash pt (open cup) 100.5C (213F). Viscosity (25): 2.07 cps
ol in water and many organic solvents.
Boiling point: bp14 96; bp400 193
Flash point: Flash pt (open cup) 100.5C (213F)
Index of refraction: nD25 1.511
Density: d424 1.04
Derivative Type: Complex with iodine see Povidone-Iodine
Use: Povidone as pharmaceutic aid (dispersing, suspending and viscosity-increasi
ng agent; tablet coating and binder). Thickener, dispersant, lubricant, film-for
ming agent and binder in cosmetics. Stabilizer, diluent, and dye dispersant in f
ood. Dye dispersant in paper and textiles. Adhesive; paper coating. Coating and
processing aid in photographic products. Manuf of plastics and rubber. Cryoprote
ctant for biological samples. Crospovidone as pharmaceutic aid (tablet binder an
d disintegrant); clarifying and stabilizing agent in beverages. Monomer as dispe
rsant and wetting agent in pigments.
Therap-Cat: Povidone formerly as a synthetic blood plasma expander. Crospovidone
as antidiarrheal.
Triprolidine
Monograph Number: 9817
Title: Triprolidine
CAS Registry Number: 486-12-4
CAS Name: 2-[(1E)-1-(4-Methylphenyl)-3-(1-pyrrolidinyl)-1-propenyl]pyridine
Additional Names: trans-2-[3-(1-pyrrolidinyl)-1-p-tolylpropenyl]pyridine; trans1-(2-pyridyl)-3-pyrrolidino-1-p-tolylprop-1-ene; trans-1-(4-methylphenyl)-1-(2-p
yridyl)-3-pyrrolidinoprop-1-ene
Molecular Formula: C19H22N2
Molecular Weight: 278.39.
Percent Composition: C 81.97%, H 7.97%, N 10.06%
Literature References: Histamine H1-receptor antagonist. Prepn: Adamson, US 2712
020; US 2712023 (both 1955 to Burroughs Wellcome); Adamson et al., J. Chem. Soc.
1958, 312. Structure-activity studies: Ison, Casy, J. Pharm. Pharmacol. 23, 848
(1971). Crystal and molecular structure: James, Williams, Can. J. Chem. 52, 188
0 (1974). Pharmacokinetics and antihistaminic effects in humans: K. J. Simons et
al., J. Allergy Clin. Immunol. 77, 326 (1986). Comprehensive description: S. A.
Benezra, C.-H. Yang, Anal. Profiles Drug Subs. 8, 509-528 (1979).
Properties: Crystals from light petr, mp 59-61. uv max (ethanol): 236, 285 nm (e 1
5300, 6800).
Melting point: mp 59-61
Absorption maximum: uv max (ethanol): 236, 285 nm (e 15300, 6800)
Absorption maximum: uv max (ethanol): 236, 285 nm (e 15300, 6800)
Derivative Type: Hydrochloride monohydrate
CAS Registry Number: 6138-79-0
Manufacturers' Codes: 295C51
Trademarks: Actidil (Wellcome); Actidilon (Wellcome); Pro-Actidil (Wellcome); Pr
o-Entra (Wellcome-Sumitomo); Venen (Tanabe)
Molecular Formula: C19H22N2.HCl.H2O
Molecular Weight: 332.88.
Percent Composition: C 68.56%, H 7.57%, N 8.42%, Cl 10.65%, O 4.81%
Properties: Crystals from water, mp 116-118. uv max (ethanol): 235, 283 nm (e 1500
0, 7400). Moderately sol in water, ethanol, methanol.
Melting point: mp 116-118
Absorption maximum: uv max (ethanol): 235, 283 nm (e 15000, 7400)
Derivative Type: Oxalate