Lately i have been running a Hasenfratz extraction of the fruits (literally) of my labor, some Peganum harmalas i have planted.
I deviated a bit from the protocol, grinding the seedpods whole ,filtering and evaporating down to a "tar/film" which i re-dissolved in brine.
Upon doing the Manske procedure two modifications have sprung into mind which im currently testing although the conditions are less than ideal*.
1)Follow the manske up to where the alkaloids have percipitated out of the solution. Improvise a waterbath ,where a volume of water is heated in a pan,a towel put in and the jar holding the solution and percipitate can rest on it without touching the metal bottom of the pan. Heat it ,but without disturbing it or mixing. Personally i heat it till the water in the pan starts emanating vapor. Then turn down the heat and let it cool there as it is,prefferably overnight. Next, transfer in fridge and let there so crystals reappear.
The idea behind it is this : By heating the liquid we redissolve some or all of the alkaloids back in solution but because they have percipitated chances are that we are going to have concentration differences in the solution of harmala alkaloids ,being more concentrated at the bottom (some diffusion might occur though).By letting it cool gradualy, in the improvised waterbath (water has better heat capacity than air) and then transfering it to fridge we aid theoretically the solution in developing bigger crystals,easier to filter.Think of it along the lines of "recrystalisation".
2)A crystal or another object could be added at the bottom of the percipitation vessel to give nucleation sites for the crystals to form. I do not know if this will work resulting in bigger crystals but it is worth a try. The object could be anything ,given that it doesnt have a totally smooth surface.
I hope the above can be tried by people more capable than me . * Due to my method of whole seedpods ,the filtering is very very difficult and i think im quite stuck at the moment. I do not have a vacuum pump to filter the solution so i cant get the percipitate.
I deviated a bit from the protocol, grinding the seedpods whole ,filtering and evaporating down to a "tar/film" which i re-dissolved in brine.
Upon doing the Manske procedure two modifications have sprung into mind which im currently testing although the conditions are less than ideal*.
1)Follow the manske up to where the alkaloids have percipitated out of the solution. Improvise a waterbath ,where a volume of water is heated in a pan,a towel put in and the jar holding the solution and percipitate can rest on it without touching the metal bottom of the pan. Heat it ,but without disturbing it or mixing. Personally i heat it till the water in the pan starts emanating vapor. Then turn down the heat and let it cool there as it is,prefferably overnight. Next, transfer in fridge and let there so crystals reappear.
The idea behind it is this : By heating the liquid we redissolve some or all of the alkaloids back in solution but because they have percipitated chances are that we are going to have concentration differences in the solution of harmala alkaloids ,being more concentrated at the bottom (some diffusion might occur though).By letting it cool gradualy, in the improvised waterbath (water has better heat capacity than air) and then transfering it to fridge we aid theoretically the solution in developing bigger crystals,easier to filter.Think of it along the lines of "recrystalisation".
2)A crystal or another object could be added at the bottom of the percipitation vessel to give nucleation sites for the crystals to form. I do not know if this will work resulting in bigger crystals but it is worth a try. The object could be anything ,given that it doesnt have a totally smooth surface.
I hope the above can be tried by people more capable than me . * Due to my method of whole seedpods ,the filtering is very very difficult and i think im quite stuck at the moment. I do not have a vacuum pump to filter the solution so i cant get the percipitate.