Not getting majority of alkaloids from first pulls

[MrAcuminata]

Gday team, I've been doing extractions for a few months now, have ended up with white crystals from acacia acuminata root bark every time but a repeat problem I'm having is that the first run of pulls (5x50ml with xylene then 5x50ml shellite/naphtha after mini a/b) are resulting in low yields, but when i use leftover soup and solvent and do a "leftovers" mini a/b I'm ending up with more fluffy white goods. I'm wondering why my first pulls from a batch are not "saturating" as much alks as possible? I'm happy to yield more from a follow up batch but would also like to save the time, effort and extra resources required and just pull as much as possible from the first attempt. Currently doing 50g cyb salt tek, adjusted NaOH to 25g instead of 50, pull with xylene 5x50ml then mini a/b those and pull 5x50ml with shellite, single water wash then freeze precip, 2 pulls per dish. Any help is immensely appreciated

 

[Transform]

Gday team, I've been doing extractions for a few months now, have ended up with white crystals from acacia acuminata root bark every time but a repeat problem I'm having is that the first run of pulls (5x50ml with xylene then 5x50ml shellite/naphtha after mini a/b) are resulting in low yields, but when i use leftover soup and solvent and do a "leftovers" mini a/b I'm ending up with more fluffy white goods. I'm wondering why my first pulls from a batch are not "saturating" as much alks as possible? I'm happy to yield more from a follow up batch but would also like to save the time, effort and extra resources required and just pull as much as possible from the first attempt. Currently doing 50g cyb salt tek, adjusted NaOH to 25g instead of 50, pull with xylene 5x50ml then mini a/b those and pull 5x50ml with shellite, single water wash then freeze precip, 2 pulls per dish. Any help is immensely appreciated

That's an interesting observation. If that were with pulls from an A/B, it would seem to imply there's something which the first pull removes preferentially, which also inhibits the solubility of DMT in the xylene. However, cyb's is more or less a STB method, so - despite all the initial freeze-thaw cycles (iirc) - it seems like it's still taking a while for the DMT to migrate out of the cellular matrix of the bark.

Do you treat the bark with a little vinegar or other dilute acid before freezing? And have you considered putting the pre-treated bark through a pressure cooker for a quick cook? The pressure cycle may help with releasing alkaloids too.

This observation could also be a byproduct of pre-saturation of the naphtha, which would initially lead to lower yields from the first pull if you were starting with fresh naphtha, then reusing the same naphtha after freeze precipitation. There's a small residue of DMT that remains dissolved in the naphtha after freeze precipitation whilh could stack up to being the missing yield from the first pull.

More than one of these factors could come into play in an extraction - or it could be something else, I'm far from omniscient

 

[doubledog]

Lye needs some time to process bark in STB.

 

[MrAcuminata]

That's an interesting observation. If that were with pulls from an A/B, it would seem to imply there's something which the first pull removes preferentially, which also inhibits the solubility of DMT in the xylene. However, cyb's is more or less a STB method, so - despite all the initial freeze-thaw cycles (iirc) - it seems like it's still taking a while for the DMT to migrate out of the cellular matrix of the bark.

Do you treat the bark with a little vinegar or other dilute acid before freezing? And have you considered putting the pre-treated bark through a pressure cooker for a quick cook? The pressure cycle may help with releasing alkaloids too.

This observation could also be a byproduct of pre-saturation of the naphtha, which would initially lead to lower yields from the first pull if you were starting with fresh naphtha, then reusing the same naphtha after freeze precipitation. There's a small residue of DMT that remains dissolved in the naphtha after freeze precipitation whilh could stack up to being the missing yield from the first pull.

More than one of these factors could come into play in an extraction - or it could be something else, I'm far from omniscient

So at the beginng of a batch I'm doing the acid soak (5% vinegar and distilled water) and hot water bath for 2 hours, reheating the bath every half hour or so then proceeding with the salt and base and repeating the heat baths for a further 1.5 hours. I haven't actually tried freeze thawing prior so that's already something to add next time for sure. After the first basification I do the 5 xylene pulls at room temp then those 5 pulls are added to a new vessel which I then add fresh room temp vinegar acidic solution to. i add roughly equal or a bit less volume of acidic solution to xylene then stir and agitate for 15 minutes or so. I then pippete off the xylene and unwanted alks and store them in a storage jar to use for leftover bacthes. I then rebase the solution with a further 25g NaOH and 200ml distilled water and stir again for 15min. I then put the solution in another heat bath and simultaneously heat the naphtha. Thus far I've had them quite hot when i combine and pull. Each pull then has a water wash in distilled water that i try to have at an equal temp to the naphtha before transferring over to the freeze precip dishes. I change water for the wash every 2 pulls. So far my biggest yield has been just under 0.5% but the end product is very nice looking white crystals. The things that stand out to me as possible issues, besides not pre treating the bark are that perhaps I'm not allowing the first base step enough time to do it's thing before i start pulling, and that maybe the naphtha pulls are being done too hot