Flash Chromatography vs CPC


#1

CPC, centrifugal partition chromatography, is a form of liquid-liquid purification that does not require solid supporting media.

I had looked into, and almost demo’d a Gilson CPC/HPLC unit earlier this year. I went with Biotage instead for initial R&D instead. Has anyone seen any Gilson units in use? The rep who spoke to me was trying to convince me that they have these units in field working with crude extract well. I was really doubting this, and their spec sheets and sales forms seemed lacking as well.
I am now getting interested, again, with purification this concept. Maybe not for pesticide remediation, but rather for cannabinoid fractionation purposes. After going through the Gilson CPC, we could recrystallize our cannabinoid fractions.

Anyone have any thoughts?


#2

I don’t have any experience either with these systems but they definitely look the most promising with production level isolation and remediation. I’ve talked to both Gilson and Rotachrom and Rotachrom seems to know way more about how to isolate and even started explaining their SOPs to me over the phone and saying that they don’t accept full payment for their systems till you’ve had proof of concept with their setup, though they are definitely more expensive. Would definitely be interested to see if anyone has experience running these systems yet.


#3

So what was the outcome of the biotage meeting? Have they demonstrated full pesticide remediation that is cost effective and scalable?


#4

Just had a through look over the Rotachrom website, and I’m even more skeptical… Just doesn’t look like the website or sales material is up to par with pharma standards, they aren’t even including device specs or anything.
Powerpoint they had looked lacking, as was Gilsons tbh.

Anyways, if anyone has seen those specs and can link me to them, It may respark my interest in CPC.


#5

Yes, they have. And in person as well. They are now also backordered on most flash units for a few months lolol. Glad we got ours in Jan.

Scaling solutions aren’t provided by Biotage directly. We have to independently source larger columns. I am going to most probably release a line of 6L and larger (3kg and larger) columns for this flash process, if enough people are interested.

Media we are using is just silica gel. We can use high performance silica if needed, but its not really. We wash the silica in an agitator tank/bucket, and flush it a few times before reuse.


#6

Yeah their site isn’t great, talking to them over the phone and email though was much better. I’ll dig through my old emails and see if I can find some specs


#7

I have been researching this alot recently and i have a stockpile of technical information like patents and white papers and scientific studies. im just a midsize SFE operation which is tiny compared to the companies getting into this market so none of my information is specific to a particular system or company. which is what i know really matters and if your talking to the companies u probably have kno what ur talking about but let me kno if you want me to put them up.
heres one
preparative_isolation_of_cannabinoids_from_cannabis-2004.pdf (5.0 MB)


#8

Reading it now. Im quoting some stuff here I find really useful for those of us with machines who can run these material tests.

"3.2.3 Thin Layer Chromatography (TLC)
Samples were manually spotted on 10x20 cm reversed phase (C18) silica gel plates F254 No.
105559 (Merck, Darmstadt, Germany) and developed in saturated normal chambers
(saturation time 15 minutes). Eluent was methanol : 5% acetic acid, 19:1 (v/v). After
development, visual inspection was done under UV 254nm. General visualization of
compounds was done by spraying with modified anisaldehyde-sulphuric acid spray reagent
[Stahl, 1967]. For selective visualization of cannabinoids the TLC plate was sprayed with 0.5%
Chapter 3
42
fast blue B salt (Sigma) in water, followed by 0.1M NaOH [Corrigan, 1980]. Reference
standards were used for identification of chromatographic spots. "


#9

yea i think we need a whole section for analytical methods that can be done outside of an analytical lab.


#10

That TLC method is MAD complicated unless it’s also attempting to quantify carboxylated cannabinoids. Firstly, 5 x 8’s are all that’s necessary. Secondly, a 19:1 MeOH:Acetic eluent is crazy. TCM will work as extraction solvent and mobile phase.

Thirdly, the modified anisaldehyde-sulphuric acid spray reagent is also totally not necessary, nor the 0.1M NaOH solution.

Spot plates. Decarboxylate. DCM mobile phase. Dip in fast blue B. Done.


#11

god dam dutch lol


#12

yea i think a big part of it is large scale purification of thca cause how else ru gonna do it


#13

lmfao I was kinda thinking thats a long ass, overkill TLC procedure.


#14

i think they do it cause they know they r gonna publish and they wanna look professional and fancy


#15

Alot of the CPC chapter was them flexing their biochem knowledge, even unnecessarily lol.


#16

Publishing data or not - What I’ve posted above is a validated, and proven method. Only reason I can see for making it more complicated is if you’re attempting to quantitatively or qualitatively detect carboxylated cannabinoids.

Perhaps they simply looked to the literature rather than the commercial sector, and only found reference to TLC methods from 1980 or before.


#17

Sustainable_Production_of_Cannabinoids_with_Supercritical_Carbon_Dioxide_Technologies_HPerrotin-Brunel-PhD.pdf (2.9 MB)
this one has some good info on some things but more what u cant do lol
the CCC is at the end


#18

Which biotage unit, 75 or 150? I priced the 150 and 400 to do this.


#19

why use CPC if your’e just going to crystallize anyway?


#20

CPC’s are like 3x the cost of a Flash system. Supposedly they use less solvent, but I would like to see a demonstration of this.