as i found more methods, here they are:
Isolation of Ibogaine from Tabernanthe iboga
In this case it was for the root/root bark of tabernanthe iboga
used as the plant material, which may contain up to 2.5 % or 6 % alkaloids respectively. The plant material was extracted with methanol four times, filtered and the methanol reduced to a small volume. An equal amount of water and acetic acid solution is added and shaken with petroleum naphtha, which is then separated and backwashed with acetic acid solution.
All the aqueous phases are combined. The aqueous phases are reduced in volume, then basified with ammonia hydroxide. This is then extracted four times with ethylene dichloride (possibly chloroform too). The solvent is washed with water, dried and concentrated. An equal amount of ethanol
is added and the whole reduced to the original volume, then about twice the amount of ethanol is added. After chilling in the fridge for two days or so, ibogaine crystallises out, and can be collected by filtration. The remaining liquid was again reduced in volume and re-chilled for a second crop of ibogaine.
Evaporation to dryness of the liquid yielded other alkaloids and residual ibogaine, which can be separated by chromatography, though can be laborious. To purify the ibogaine 100 mg of the crude ibogaine, as obtained above, was dissolved in 1 l of acetone, then 53.1 ml of 1:1 HCl was added, with ibogaine HCl precipitating (108 mg in this case) out straight away, this compound being relatively insoluble in acetone, compared to the base. Isolated by filtration.
ibogaine mp 151-153* C sol - ethanol, ether, chloroform, acetone
ibogaine HCl mp 299-300* C.
In tabernanthe iboga, ibogaine seems to be the most active and prominent alkaloid
. In other species that are recorded as containing ibogaine, other alkaloids sometimes make up the majority of the alkaloids, with ibogaine being a minor component. Many related alkaloids however have a similar but not such strong action as ibogaine. The isolation of ibogaine from more complex mixtures of alkaloids may be a bit more tricky, especially if ibogaine is not a major component of the alkaloids.
Extraction studies of Tabernanthe iboga and Voacanga africana
Extraction of T. iboga
root (TA). One kg (2.5 L) of powdered T. iboga root and 5 L of 0.5% acetic acid were placed in a 6 L plastic bucket, stirred occasionally for one hour, and filtered through a cloth sack. The sack was wrung to expel all possible liquid from the root powder and the filtrate (pH = 3-4) was basified using 60 mL of 30% ammonia. The resulting flocculent, medium greenish-brown precipitate of TA was patiently gravity filtered through 30 cm filter paper and thoroughly rinsed with distilled water. This procedure was repeated twice more on the same root powder. The filter papers bearing the TA were placed on paper towels on a wire rack and left in a warm draft until successive weighings detected no more than 0.3% loss per day. The hard, dark brown solid weighed 30.037 g (3.0%) and was ground in a mortar and sifted to give a fine brown powder.
Conversion of alkaloids to the hydrochlorides (PTA HCl). 28.00 g of powdered TA was placed on a filter paper in a funnel and 450 mL of acetone was added in portions with gentle stirring. The funnel was removed and 2 mL of concentrated HCl was slowly added dropwise to the flask with swirling, occasionally adding a trace of PTA HCl from a previous batch to initiate precipitation. After waiting a few minutes to allow precipitation to begin, dropwise HCl (2.8 mL) was added with swirling until the liquid became acidic according to pH paper. A final 0.4 mL of HCl was added dropwise and the flask was placed in the refrigerator overnight. The yellow powder was scraped from the sides of the flask, filtered, rinsed with 84 mL of acetone, and dried at room temperature to give 9.493 g (33.9%) of PTA HCl. The black, spent TA weighed 14.521 g (51.9%) after drying.
Ibogaine HCl. 9.712 g of PTA HCl was patiently dissolved in 150 mL of boiling 95% ethanol, set overnight at room temperature, refrigerated for two hours, and the mother liquor was decanted from the yellow crystals (4.412 g). Recrystallizing again from 80 mL of 95% ethanol gave 3.666 g of mostly pure ibogaine HCl.
Recovery of residual alkaloids (RA). Most of the acetone was distilled from the filtrate from the preparation of PTA HCl and the remainder was evaporated using a stream of air. The dark residue was dissolved in 400 mL of distilled water, filtered, and basified to pH 9 using 3 mL of 30% ammonia. The medium yellow suspension was filtered through a fresh coffee
filter paper and left on a warm surface to dry. The chunks of light, chalky, off-white alkaloid residue weighed 4.750 g (17.0%).
Extraction of V. africana trunk bark (VTA). One kg of powdered trunk bark was extracted in the same manner as the T. iboga root above, resulting in 59.723 g (6.0%) of crumbly brown voacanga total alkaloids (VTA).
Conversion of alkaloids to the hydrochlorides (VPTA HCl). 75.00 g of VTA was treated in a manner similar to the PTA HCl above, resulting in 35.929 g (43.6%) of medium brown VPTA HCl. The spent VTA weighed 31.534 g (42.0%).
Recovery of residual alkaloids. The filtrate from the preparation of VPTA HCl was treated in a manner similar to the PTA HCl filtrate above, resulting in 12.119 g (16.2%) of chalky, off-white solid.
Preparation of V.Africana Extract
Total alkaloidal extracts of Voacanga africana
seeds (obtained from Valley Farms Ltd, ccra, Ghana) were preparedusing standard extraction procedures [10,43]. Brieﬂy, dried seeds were powdered and defatted using petroleum ether, and a crude concentrated extract was obtained by a series of ammonia basiﬁcation and methanol extractions. This crude extract was then puriﬁed using solvent extraction, pH manipulation, and precipitation techniques .
Used and Their Sources Pluronic F127 was obtained from BASF Wyandotte (Michigan); 6-cyano-7-nitroquinoxaline-2,3-dione (CNQX) was obtained from RBI, while ibogaine, bicuculline, nystatin, haloperidol, and all the salts in the ACSF were obtained from Sigma (St. Louis, MO). Stock solutions of ibogaine and VA extract were made in 63% ethanol and diluted 500 –1000-fold prior to application.
Ibogaine from Trachelospermum jasminoides
"Leaves and stems (50 kg) were dried in the shade and extracted with ethanol. The crude alcoholic extracts were concentrated and partitioned between 10% hydrochloric acid and chloroform (pH 1). The chloroform layer was dried with anhydrous sodium sulfate and concentrated to a gum (25 g, F1). The aqueous acidic layer was basified with aqueous ammonia and extracted into chloroform at various pH values (5, 7, 9, and 11). The fraction obtained at pH-5 (20 g, F2) was found to contain major alkaloids. We have recently reported five indole alkaloids from this plant (2)."
"The crude alkaloidal fraction (F1, 25 g) was subjected to flash chromatography. [...] The alkaloid isolated was identified as voacangine-7-hydroxyindolenine by comparison of its spectral data with those reported in the literature (3). [...] Voacangine-7-hydroxyindolenine may have been formed by air oxidation during the extraction and isolation process."
"Fraction F2 (20 g) was also loaded on a silica column (750 g) and was eluted with increasing polarities of mixtures of petroleum ether, chloroform, ethyl acetate, and methanol." "The fraction obtained on elution with chloroform:ethyl acetate (3:1) consisted of a mixture of four alkaloids. This fraction was subjected to a flash chromatography which was eluted with increasing polarities of mixtures of petroleum ether in acetone. The fraction obtained on elution with 70% petroleum ether in acetone was found to contain two major alkaloids. These alkaloids were separated by preparative TLC on silica gel (petroleum ether:acetone:ammonia, 6:3.95:0.05). The faster moving alkaloid was identified as ibogaine by comparison of its spectral data with those reported in the literature (7) while the slower moving alkaloid was identified as tabernaemontanine (8)."
"Further elution of the same column with 60% petroleum ether in acetone afforded another alkaloid which was further purified by preparative TLC on silica gel (petroleum ether:acetone:ammonia, 1:1:0