Process for removing pesticides from ginkgo biloba extracts, and extracts obtainable by said process
a technology of ginkgo biloba and extract, which is applied in the direction of separation process, immune disorders, extracellular fluid disorders, etc., can solve the problems of cross-contamination of pesticides originating from nearby, unfavorable and inability to rule out unlawful or improper use of substances
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example 1
Purification of the Extract Produced According to Example I in U.S. Pat. No. 5,700,468 and EP 0 360 556 (Indena)
[0021]1) 100 kg of chopped leaves is extracted 4 times with 400 l of 60% (w / w) acetone at a temperature of approx. 50° C.
[0022]2) The combined percolates are extracted in countercurrent with 500 l of hexane.
[0023]3) The defatted solution is concentrated under vacuum to a volume of 200 l, left overnight at 2° C., and then centrifuged to separate the biflavone fraction.
[0024]4) The aqueous solution is extracted in countercurrent with 400 l of an 8 / 2 v / v mixture of n-butanol / toluene.
[0025]5) The organic solution is concentrated under vacuum to a small volume, substituting with water. The concentrate is taken up with water to obtain a solution with approx. 30% of dry residue.
[0026]6) The solution is extracted in countercurrent with approx. 65 l of ethyl acetate. The aqueous phase is concentrated to a syrup-like consistency and dried under vacuum, to obtain an intermediate enri...
example 2
Purification of the Extract Produced as Described in Example II of U.S. Pat. No. 5,700,468, EP 0 360 556 (Indena)
[0037]1) 100 kg of chopped leaves is extracted 4 times with 400 l of 50% (w / w) methanol at the temperature of approx. 35° C.
[0038]2) The combined percolates are concentrated to 100 l under vacuum at 40° C., the concentrate is taken up with 100 l of methanol, and the suspension obtained is filtered.
[0039]3) The filtered solution is extracted 3 times with 100 l of a 9:2 mixture of toluene / n-butanol.
[0040]4) The combined organic phases are counterwashed with 50 l of 50% methanol.
[0041]5) The water-methanol solutions are concentrated under vacuum to an aqueous solution and, after filtration, are extracted with an 8:2 mixture of n-butanol / toluene.
[0042]6) The organic solution is counterwashed with water and concentrated under vacuum to a small volume, substituting with water. The solution is taken up with water to obtain a solution with a dry residue of 20%.
[0043]7) The result...
example 3
Purification of the Extract Produced According to Example I in EP 431 535 (Schwabe)
[0054]1) 100 kg of chopped leaves is extracted twice with 750 kg of 60% (w / w) acetone for 30 mins at the temperature of 57-59° C.
[0055]2) The combined extracts are concentrated to an aqueous solution with a dry residue of 30-40%, an equal volume of water is added, and the mixture is left under stirring for one hour at 12° C.
[0056]3) The alkylphenol-rich precipitate is separated by centrifugation and eliminated.
[0057]4) 30% of ammonium sulphate is added to the clarified solution under stirring, and the solution is extracted twice with half a volume of a 6:4 mixture of methyl ethyl ketone / acetone.
[0058]5) The combined methyl ethyl ketone / acetone solutions are concentrated under vacuum to a dry residue of 50-70%, and then diluted with water and 95% ethanol to obtain a 50% ethanol solution with a dry residue of 10%.
[0059]6) An aqueous solution of lead hydroxide acetate is added under stirring until the co...
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