High Purification S.O.P.

Here we will find the collective testing and collaboration between Summit Research users and advanced testing personnel for the validation of a streamlined high purification standard operating procedure for quality results.

These results were validated throughout the user base with both processing and analytical testing of batches that have confirmed their results.

Steps are somewhat repeated from last articles, it is the series of hardware used in the series of pre-processing that makes a significant difference. This is for high purity/potency results. This is not directed to a 1 step process that yields somewhat larger or “dirtier” results. This also will address the degradation factors in other processes with a collective solution through hardware selection and use.

• Winterization of product. Work within the 3 step temperature/winterization filtration process to ensure impurities are removed at various temperatures. Start with slightly cold, then go colder, then go deep cold overnight. Each step will remove more of the mass from the solution making lower temperature coagulation rapid and efficient, as well as faster flow each time the solution is filtered at desired temperature.
• Now do a carbon scrub at warm temperatures around 38°C or so. This is very basic, you will need carbon powder and silica for bedding to properly remove the carbon powder, dyes and other related compounds the scrub is tailored to take out.
• Rotovap your product down.
• Remove all water, alcohol, terps and related azeatrope through a sealed chamber/reactor while diffusing nitrogen gas through the mixture. Your fluid will need to get to around 140°C to ensure all volatiles within that range are removed. This can be done on a hot plate. Take note that to ensure a reduction of any degrading effects, you will need to use the nitrogen as a basic gas scrubber which will help flow vapor upward and out.
• Begin a distillation, use any of the SPD-1, 2, 5 or 6 standard systems. This will now be referred to as a first pass. Within this first pass you are aiming at removing all the compounds that are targeted at a fast paced effort while trying to retain 85-90% or above. It is to be noted that you are still removing heads, body and tails appropriately like normal. (Pictured above example of heads) The difference here is the temperatures offer a high flow process, not a tuned one. When diving down to the molecular bandwidth desired you can only target a certain band. Example for targeted section of compounds for first vs second pass theory:

1. 1. Original oleoresin + 400 chemical compounds.
   2. Winterized + polished scrub = 200 chemical compounds.
   3. First pass narrowest band 80 – 100 compounds.
   4. Curative compound range available estimate 50 chemical compounds.
      ****As you can see we are only able to retain a band of 80-100 within the first targeted while being concerned of abut 50.
   5. First pass reloaded material with available range of 80-100 compounds.
   6. Second pass narrowest band 55-70 compounds(closer to 55-60).
   7. Example curative compound range estimate 55-65 chemical compounds.

• This exact theory above is related to most documented literature, this was a basic simplified explanation and none of those numbers are actually to be noted. They are examples or separation theory to actual performance in short path distillation. It is to be noted with the entire fraction collected (no separation of heads and tails) which is effectively the operation of a wiped film extractor; will yield a much much higher chemical compound bandwidth, and with these next steps we are going to explain the process to mechanically remove the most available-unwanted compounds.
• At this point the first pass has been done with a “roughing pass” using the basic SPD series designed heads. The results from the main body should be collected with other main bodies, and the tails will be left in a beaker with other tails. The tails are to be processed differently but for the nature of this SOP we are going to be working with a collection of main body 85-90%+ material. If it’s not in this range the next steps will still work, and with considerable results but not to the highest degree.
• Take the product from the first pass and dissolve it from a 1:1-1:4 ratio. This is variable to the material but we feel starting at 1:1 is fine. The dilution will be a solvent that is highly non-miscible with water, in this case you can use hexane. If your first pass was 1000ml, then add that to 1000ml of solvent. Allow to mix down, and it is wise to use temperature to fully dissolve the solution. Be very careful as hexane is more flammable than alcohol.
  1. 1. In this example you will have 1000ml first pass + 1000ml hexane; considered your 2000ml solution dissolved load amount. Due to the density per ml variance between hexane and extract, your solution load amount in reality will be a lot less than 2L, something around 1700-1800ml. For instruction purpose we will consider this out 2000ml load. This is why we are recommending the use of a 4L separatory funnel for this process. In large scale solution you would use a 20-50 liter glass reactor.
     2. A pre-step to this process is by taking a 20 gallon ice bucket (or ptfe trash can) and preparing a highly saturated salt water solution. This is done by adding 25-30% in volume rock salt easily found for water softeners to the can, and adding hot/clean water. Stir it with something until salt dissolves, and add more if needed until salt stops dissolving. Allow this can of salt water to cool back to room temperature. You now have salt water prepared for the washes, it will take A LOT, so don’t be shy making up more than you need.
• First step is to put the 2L load solution of hexane in the sep funnel. Now add the same volume in salt water. Shake up but keep cap on tight, when done shaking carefully burp the funnel. If done in a reactor just leave one port open for venting. Shaking is enough to visually see a small bubble/slight foaming occurring. Now allow to sit. The solution should separate completely for first pass product within 2-5 minutes.
• The separation has occurred, the water should be dirty. The salt water will also be at the bottom and the hexane solution will be at the top. Drain the salt water layer out right up to the hexane line.
• On the second to fourth pass you will considerably see the salt water become more and more clear. This is removing water soluble compounds from the layer. Even if you see clear water by the third wash it doesn’t mean anything. You are now going to be focusing on the distance right between the two layers. Even if the salt water main portion looks clean; you will see a “rotten jelly” like film and presence between the two layer. Now upon every wash you will be focusing on this section. When you DO NOT see anything in between these layers, you are now pulling water soluble pesticides. This process should continue for about 2-4x times after you last see anything in between those layers to be sure you have dragged as many compounds as possible.
• The next step is costly and expensive, and in some cases you need to add more hexane through the last filtration flush. After removing the water from the last separation, you are going to drain off the hexane solution and put it off to the side. You can now clean the sep funnel and put it away. The next step is to prepare a magnesium silicate 60a bed, similar to a silica scrub with carbon. Instead, you are going to make a bed with 60a and a solution of hexane slurry,  no alcohol. When you are ready with hexane solution containing 60a pour this into the Hochstrom, or a narrow Chromatography Column. The taller the bed the better, but for “flash response” this can be done similar to silica/carbon scrubbing, other than more surface thickness for the bed is desired.
• Gently apply vacuum to your collection bottle. Pour your salt water washed hexane solution over it, and allow the 60a to do its thing and absorb what it wants, while the curatives flow through, you will see a considerably high change in color, and some yields will be lost. This step can be bypassed after the hexane salt water wash if the end user is asking for a higher yield, however this will remove a considerably large chunk of pesticides if not all of them(nothing is 100% all); the color will be near non existent, and the potency will go up from the ability to remove compounds that would otherwise boil off at the same rate as your curative layer. This specific step is a selective wash and sometimes you need to take cold hexane and pour it over the best right when the best starts to go dry, this will take any remainder curatives down with it while leaving all the stuff the 60a media wants to adsorb. The media is expensive and complex to reuse, effectively you’ll need acetone and then removing it and roto it down to a dry powder. Some of these media can not really be reused as its effective relationship to adsorbing the GUM from the product and more colors has been achieved.
• Now you can rotovap down the hexane and remove the ultra polished oleoresin and place it in your distillation apparatus to perform a dialed in short path process.
• The next step is using a variation of glassware to properly distill out this prepared product. The standard SPD series heads can be used (SPD-1, 2, 5 or 6 setups). We have seen a higher retention of potency on a consistent basis using the standard e-vigoreux design heads. Unfortunately there will be a 2-5% maximum shift from the delta9 content to the delta8 range. Unlike other packable methods and heads out there, ours has a superior performance curve and low gradient for the core of the packing.
• To perform a packable head process it is relatively the same as standard. The packing section will first be loaded with 8×8 raschig rings as a bed. Then, 6×6 raschigs on top of that. The larger allows a hotter flow rate while creating a considerable discharge effect compared to the smaller rings which focuses on retention and rejection. These SPD-x.1 thermal+ series heads (example SPD-5.1) with summit desired methodology of packing and pre-processing out performs any of the products on the market due to its highly efficient packable material location. The ability for random packing rejection in the path is normally overshadowed by operational characteristics with other systems that simply are not built to perform.

Video date Feb 6, 2018