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Repeated Extractions of MHRB, comments on yield and color per extraction

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La Alquimista

Rising Star
A recent extraction was performed using Cyb's Max Ion Tek as a guide, following instructions exactly with 50g MHRB. Extraction (using 50mL naphtha each time) was performed with 50mL quantities naphtha 10 times. Extractions 1-7 were collected together then 8, 9, and 10 separately to determine yield per extraction.

Freeze precipitation was performed and product was collected by vacuum filtration. Product from extractions 1-7 was yellow crystals with a distinct odor. Product from extractions 8, 9, 10 were white cyrstals with no odor. The following amounts were obtained after drying 24 hours:

1-7: 430mg
8: 40mg
9: 80mg
10: 80mg

Net yield 1.26% by mass from starting plant.

After obtaining these results it is now questioned why Cyb's Max Ion Tek specifies to perform extraction 7 times. It seems about the same mass of product is obtained for each extraction 1 to 10 and another 10 extractions could yield useful quantity further product. Has this been observed by anyone else and how common or expected is this result?
 
In Cybs original tek (Hybrid salt tek) he states "keep pulling till that bark looses its bite". I pull until it becomes obvious there is no more to be had. When yields per pull are slowing down I heat the motherliquor and solvent in simmering water till hot to the touch.
 
It is clear additional extractions will be to benefit for total yield. The base solution and bark has been retained in a storage vessel for several weeks and in the next work, another 10x extractions will be performed followed by another two sets of 5x extractions, and the yields to be reported.

It seems inefficient to evaporate and freeze precipitate each extraction individually since such further yield is still possible - do you perform individual extractions and compare yield per unit on all extractions, or on larger volumes suppose 5x or 10x? Does the addition of heat to aqueous layer allow further extractions by nature of heated aqueous layer, or is this a result of accelerated dissolving of plant material? Perhaps leaving the solution in a hot bath for some days would be to benefit, though it has been read at some point this causes breakdown of product into oxide form.

It will be interesting to see what yields are after the plant matter has been sitting in NaOH + water for some time.
 
At last La Alquimista has obtained the proper supplies for naptha extractions. Turkey baster lead to much struggle.

In previous work (see OP) 10x extractions were performed with a yield of 630mg from 50g starting material. Recently an additional 10x extractions are performed with yield of 180mg, finally an additional 2x extractions are performed with some crystals visible in soln reduced to 40mL, however not enough to conclude further extractions are to be worthwhile - at best several mg by visual estimate.

Final yield on 20x extraction with naptha is 810mg or 1.6%, consistent with expected yield from root bark. This suggests 20x extractions is enough to get expected results.

It might be valuable to perform an additional 10x extractions to be sure this conclusion is reasonable, time will tell. It would be shameful to waste additional product down the drain.
 
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