Homogenized micro-emulsion vs. sonicator toll processor for nano-emulsion

cbd-distillate
nanoemulsion
homogenizer
cbdisolate

#1

Hello everyone!

With the help of this community, we have been making some awesome CBD distillate and I feel like we have a pretty good grasp on it. Now we are trying to decide how to further process our distillate into products.

Our dilemma is this: we can toll process our distillate or isolate (we are going to play with crystallization in a bit) on a local sonomechanics machine for a steep price - $10-18/g depending on quantity processed, including emulsifier and any other reagents. Even at that price, having a water soluble product is highly profitable when sold at retail and can be used in a variety of products; however, we are also considering just getting a high quality homogenizer from @CATScientific and going the more traditional emulsion in carrier oil route and making products in house.

This is what we are stuck on:

  1. Should we just buy a homogenizer? Financially it makes sense, we can buy a homogenizer for the price of tolling <100 grams of material. The end goal is liquid capsules, tinctures, and single dose water soluble drops. Also, possibly food items, like gummies or cookies or something. I have read through Turning THC & CBD Water Soluble a few times and I’m not sure if the homogenizer alone can get us totally water soluble. @ShearGuy - are your results soluble and stable in aqueous solution?

  2. At what point is sonication a necessity, if ever?

  3. I haven’t found any peer-reviewed articles to back up the nano-emulsion bioavailability claims for CBD. Is this bullshit? Or does sonication truly produce a superior product?

Thank you for any information/advice. I’m starting to think that the homogenizer is the way to go, but I’d like to clear up these final sticking points before making a decision.


#2

The choice of method and emulsifiers is dependent on what characteristics you are looking for in an end product. If you want to make a clear “enhanced water” sort of product you will need particles smaller than the wavelength of visible light. The only 2 methods I know of that will achieve this are high pressure piston homogenizers such as a Microfluidics or Gaulin. These are hugely expensive, energy hogs and repair prone. The other is sonication with it’s own drawbacks of low throughput and high cost. If you are making chewables or tinctures etc, a rotor stator device is the way to go. If however you think you can charge a higher price for a nano-emulsion just because it’s “nano” that has to be considered. With regards to bio-availability etc., there are people who think its instantaneous and others who think it is so much marketing woo. My own opinion is that it comes too close to making a claim that invites FDA scrutiny, whether health claims or manufacturing under cGMP conditions.


#3

nano definitely hits harder

I am in a similar boat, I own a Cat Homogenizer and still working on a syrup recipe


#4

It is possible to make a thick syrup that is indefinitely stable with only a shear homogenizer. If you try and dilute it into a thinner beverage the emulsion will degrade over a few days time. Then you require more powerful homogenization.


#5

From what I understand sonication is the way to go for making emulsions.

https://www.hielscher.com/ultrasonic-cannabis-oil-emulsion.htm


#6

My results using a Polytron and gum Arabic have proven to be soluble and stable so far. I am doing a long term stability test on the syrup dissolved in water. These are standard beverage industry tests, the “ring test” looks to see if the particle size is too large to stay fully dispersed or too light and floats to the top. The creaming test looks for free oil floating on the surface that indicates the oil phase was not fully emulsified.


#7

I own a Hielscher and the throughput with the unit I have, the UIP500 with the flow through cell a holding tank, pump and chiller is pretty dang good. It can easy handle 2L/min and a max of 4L/min. Designed to run 24-7 that means it can make 760 to 1521 gallons a day of a concentrated emulsion for an investment of under $15k. At a concentration of 10mg/mL it pays for itself quickly. In addition to emulsions you can very easily extract with this setup straight into mct, olive oil, glycerin, coconut oil, ethanol or other solvents making it perfect for so many products. Anyway getting a high quality emulsion does require a fair bit of R&D and one with minimal to no nasty surfactants will be much easier with a nice sonicator.

If the end product goal is to produce high quality liquid based products that are shelf stable and have a better onset time I’d go with the Sonication. Start saving for your own.


#8

Thanks,

I guess I had been thinking about scaling up from the lab sized units. Good information.


#9

ShearGuy, what ratio of gum arabic are you using?


#10

From my gum supplier:_“You will need 3-5 parts gum per 1-part resin. They will require being placed under high shear for 20-40 minutes. To make up a concentrate, we recommend hydrating the gum acacia for 2 hours in water (or 45 minutes for pre-hydrated gum acacia and modified gum acacia), adding your resin under high shear (20,000 RPM) and letting this run for 30 minutes…You will only be able to get a 5-7% resin emulsion while using traditional gum Arabic and up to 10% with the chemically modified gum Arabic.”

I run a Polytron at 30,000 rpm with an ultrafine generator and need about 15 minutes.


#11

Excellent, thanks for the info!


#12

Thanks for the input everyone. I’m going to get some quotes from Hielscher and see if they have a smaller scale unit that will work for us. I think “nano” branding could be a good way to differentiate some of our products.

In the meantime, a friend of mine saw this post and has the CAT x1000 homogenizer. He offered to let us borrow it, so we will play with that and see how it goes. I’ll use what @ShearGuy has posted as a starting point. I’ll post updates/pics of our results to this thread!


#13

To get the final emulsion into a softgel, like the CBD product pictured here, is it possible to do it without expensive equipment or utilizing a third party?


#14

As far as I know, there’s no easy/cheap way to manufacture softgels. You’re better off going with hard gelatin capsules, preferably with a carrier like MCT that is not really liquid at room temperature and won’t leak.


#15

Direct sonication leaks heavy metals into your product- if you go the route of sonication for a consumable product you have to invest in the v expensive indirect sonicator equipment.


#16

I use the Hielscher 1 kW with a special add-on for injecting the CBD. It uses 48 small needles in the reactor. I had my emulsions analyzed for stability and size. All came out at 10 to 15 nano meters and were stable for ever.
This special needle thing is called MultiPhaseCavitator Insert or InsertMPC48. Gotta love German ingenuity. The whole unit is an incredible engineering marvel


#17

Just curious if you used the CAT X1000 homogeinzer to process the emulsion?


#18

Like I just said- if you are directly sonicating your product you are leaking microfine nanoparticles of heavy metals into your product and harming your customers- get yourself set up with an indirect system.


#19

Where are the heavy metals coming from? The reaction vessel? I 100% guarantee a 316L SS vessel will not leach metal nano-particles into solution.


#20

This is a really good answer.

The piston-type homogenizers are indeed a large investment and power hog. However, you can process at pressures up to (and potentially beyond) 10,000 psi. You essentially shoot this stream at a plate of extremely hard material, like tungsten carbide, and the sheer stress reduces your particle sizes immensely.

I would say, to reach a nano-scale emulsion you’ll need to post-process homogenized materials even further (perhaps with a refrigerated centrifuge).