Decoding The Holy Grail: Terpene & Cannabinoid Retention: Decarb to Extraction

[Oldbear]

OB, Thanks,
Were your samples FH or dried buds?
What did you use for time and temperature?
Did you grind your material?
Did you stir it a lot?
Want me to ask more questions? [;>)

The samples were 'as shipped' from a Canadian licensed producer. They are dried so will have already lost terpenes. So all the more reason to minimize further loss during decarb.

I dont grind the buds, but do use fingers to crumble it into tiny bits.

Ive been following a 110 minutes @ 220F baking time. I use a toaster oven and have confirmed the temperature with a laser temperature tool.

I didn't stir it while it was in the oven because I didn't want to remove that lid. What I do, after decarb, is put on the proper lid while the mixture is still hot. This creates a vacuum seal once it cools. Once the lid is on, I give it a good shake to stir things up. If any terpenes or cannabinoids have attached to the glass, Im hoping this will get it back into the solution.

Then in to the fridge for curing and storage. Ill give a new batch a shake every morning, allow it to come to room temperature during the day, then a shake and back in the fridge overnight. I do this for 1 week then it just stays in the fridge.

Final step is to separate the oil from the plant material using a fine mesh strainer. (I warm it up to around 180f so it flows easier) Then in to a glass bottle with a dropper or into capsules. I keep the oil soaked plant material - use it for baking or Ill eat it.

Questions are always welcome

 

[Oldbear]

I had some interest in it so was poking around the tcheck site. What Ive read:

The test result comes out as a single number.

Once you press “GO”, it takes under 45 seconds to get the CBV, or aggregate herbal Compound By Volume reading. Use the tCheck Web App to assist in adjusting your recipes and determining herbal compound type.

Two other fine print points from their site - the tool is rated at +/- 10% and there are max limits depending on the base. For example an olive oil solution the analysis max is 15% so anything stronger wont show up.

 

[Canyon]

I had caught the +/- 10% and missed the 15%.

The 20% window of error can probably be narrowed by mixing a known concentration of an extract like BHO in the same oil used for the infusions. Then, use the difference between the math and the tCheck as an offset for the test results.

Extracts are down to about $70 a gram. They test around 67 to just under 70%. I should be able to get a gram for the cause while I am in Albuquerque. This could be a reasonably accurate way to test home extractions. It's not like the infused oil will be wasted.

If the tCheck could test THCA, CBDA THC, CBD and CBG it would be a lot more useful. Even so, I keep thinking of ways to use it.

I never know

 

[Oldbear]

... always pondering about things.

I wonder if a good calibration / precision test might be to run (for example) 3 tests on the same sample. Just to see if they are the same, or not.

 

[Kicknitup1]

Kickn, I have been to the tCheck site several times. Could you describe what it actually displays as results? I am thinking that it is including the acids in the total.
[/SIZE]
I never know[/QUOTE]

Yes. It only measures total cannabinoids. It's handy but not perfect. But, as far as I know, it's the best thing out there. It's helpful to know your starting material. Usually most of us do not have that luxury. However, this time, WE DO KNOW the properties of the starting material. That is why this round is going to be so meaningful. We know what we started with and we will measure what ends up in the oil. Then we will know what we are losing along the way and hopefully, where we lost it.

For instance, we know the Nightmare Cookies has a whopping 23% thca! No thc, no cbn and surprisingly no cbd or cbda. So, in a perfect world, we would get 20.24% thc per gram of starting material into the oil. So that would be 202 mg thc per gram of starting mtl. I am certain that it will not all end up in the oil. Our job is to quantify what does get extracted and at what points we lose thc along the way. Isn't this exactly what everyone has been dying to know??? Oh yeah baby!

 

[I8myweedie5]

Decarboxylation Study of Acidic Cannabinoids: A Novel Approach Using Ultra-High-Performance Supercritical Fluid Chromatography/Photodiode Array-Mass Spectrometry (PDF Download Available)

Marijuana Growers HQ – Decarboxylation: Marijuana Alchemy

Skunk Pharm Research

Patent US20120046352 - Controlled cannabis decarboxylation - Google Patents

Extraction of pharmaceutically active components from plant materials - GW Pharma Limited

Taming THC: potential cannabis synergy and phytocannabinoid-terpenoid entourage effects

Cannabinoids as Therapeutics - Google Books


above are all fantastic links for info on not only decarboxilation but many more things as well. some are studies or reference studies doen in labs, while others are experiments from the home. i realize that not all info presented in about decarb, but it will be related in one way or another. and yes its a ton of info/. not for the faint of heart, but this is some of the best info ive found on the matter. hope it helps!!!!!!!!! im currently reading it all as well . i believe with all this info, anyone can learn to do a near precise decard for any cannabis application

 

[Kicknitup1]

I had some interest in it so was poking around the tcheck site. What Ive read:

The test result comes out as a single number.

Once you press “GO”, it takes under 45 seconds to get the CBV, or aggregate herbal Compound By Volume reading. Use the tCheck Web App to assist in adjusting your recipes and determining herbal compound type.

Two other fine print points from their site - the tool is rated at +/- 10% and there are max limits depending on the base. For example an olive oil solution the analysis max is 15% so anything stronger wont show up.

I don't know where the 20% # came from. The device is accurate to +-10%. It will measure up to 15% concentration of olive oil carrier. If your concentration is stronger than 15%, it will say "over". You have to dilute and retest.

 

[Canyon]

Quick question, would the terpenes be included in the CBV total?

If have it correct there is a 12% loss of weight in the decarb conversion to consider. If you test after decarb you will get the computed values (THCA x 0.88 + THC = Decarboxolated Value of THC). That may account for some of the loss you are experiencing.

Kickn, the 20% came from +10%/-10% margin of error for the MBV reading. It did look a little funny when I reread it.

Oldbear, even the lab guy averaged three samples with the quick test they have. Thanks.

i8, That is some good info. I copped it to a word document. The moderators tend to limit what they allow links to. They may edit them out. If they pull them, you will get an email. It is probably a good idea for anyone to copy them while they can.

 

[Kicknitup1]

I had some interest in it so was poking around the tcheck site. What Ive read:

The test result comes out as a single number.

Once you press "GO", it takes under 45 seconds to get the CBV, or aggregate herbal Compound By Volume reading. Use the tCheck Web App to assist in adjusting your recipes and determining herbal compound type.

Two other fine print points from their site - the tool is rated at +/- 10% and there are max limits depending on the base. For example an olive oil solution the analysis max is 15% so anything stronger wont show up.

I don't know where the 20% # came from. The device is accurate to +-10%. It will measure up to 15% concentration of olive oil carrier. If your concentration is stronger than 15%, it will say "over". You have to dilute and retest.

 

[I8myweedie5]

canyon, thanks for that info, didnt know that they would take that down. if all is lost i took a picture of it and can re visit the websites and give people links over private email if necessary

 

[Bucudinkydow]

Thanx, folks, for initiating this study. Anxious to ride along.

 

[Oldbear]

Came across this today:

What Does Drying Buds Do to Terpenes? – High Times
Sirius J
4-5 minutes

Over at the University of Mississippi, the only place in the United States that’s legally allowed to grow pot as far as the federal government is considered, they’ve been doing research on cannabis since 1968. Most of that research aims to reinforce the federal government’s stance on marijuana, but that doesn’t mean there’s not room to take advantage of the knowledge they’ve been gathering.

One such study they submitted in 1995, The Volatile Oil Composition of Fresh and Air-Dried Buds of Cannabis sativa, is a perfect example. According to the authors:

The recognition of the smell by law enforcement officers has recently been challenged in courts by the defense in criminal cases. The purpose of this paper is to identify the major components of the essential oil of cannabis and to study the effect of drying and storage of the plant material on the stability of the characteristic components of the oil odor.

An interesting premise, but their findings give growers and extract artists the opportunity to look at what exactly drying and curing do to the terpene content of our favorite plant.

So here’s what they did: They harvested 60 grams of buds from the same plant and grouped them into four categories of 15 grams each: one was kept fresh (A), the second was dried at room temperature for a week (B), the third was dried at room temperature for a week then stored in a brown paper bag for one month (C), and the fourth was dried for a week then stored in a brown paper bag for three months (D). The four allotments were steam-distilled, and the resulting oil was analyzed chemically and a yield was calculated for each. Steam-distillation extracts just the oils (terpenes) that give cannabis its smell, and nothing else.

The major components were myrcene (hoppy smell) and limonene (citrus smell), with linalool (lavender, citrus smell) and caryophyllene (strong peppery smell) being relatively significant players as well. Fresh buds obviously had the largest terpene content, but only during the first week did most of the terpenes evaporate; after that the terpene loss plateaued.

Their findings show that drying changes the relative concentration of terpenes in the oil. Smaller, lighter terpenes (monoterpenes) like myrcene and limonene evaporated faster. Bigger, heavier terpenes (sesquiterpenes) like caryophyllene don’t evaporate as quickly, and represent a larger percentage of the oil after drying.

In summary, if you want the full terpene content in your oil, extract it from fresh frozen buds, but keep in mind that moisture in the buds prevents the butane from dissolving everything it needs to dissolve.

If you’re going to dry the pot, you might as well dry and cure it all the way because most of the terpenes are lost during the first week, and the loss stabilizes after that. The terpene loss isn’t homogeneous; drying will likely lead to a more peppery-smelling oil, since caryophyllene will make up a larger percentage of the oil. There will be considerably less myrcene after drying, but limonene stays relatively constant.

Both myrcene and caryophyllene hit cannabinoid receptors, so different proportions of them will also change the psychoactive effect of your oil. How exactly do they affect the high? We don’t know yet for sure, but we hope to do some experiments in the near future.

What were the findings for the researchers at the University of Mississippi?

To evaluate the odor of the different oils, technicians experienced with marijuana smell were asked to identify the smell of the individual oils. The subjects were able to recognize the smell of all oils as that of marijuana.

They all smelled like weed. What a fascinating conclusion.

 

[Kicknitup1]

Nothing says science like storing in a brown paper bag waiting for the majick to happen. lol Right beside the banana ripening study.

 

[Kicknitup1]

Wow Canyon, was that your seeds you got out of a bag of weed way back when? 29% thca????

 

[qaza]

I'm in too, this will be so interesting

 

[Bucudinkydow]

Interesting article, oldbear. Thanx. I've been making ethanol tinctures for the past year. Irrelevant of the strain I use, I'm getting more of a sedative experience than I would prefer. I understand the personality of cannabis is due to the terpenes so I'm on a quest to create a tincture while maintaining the highest level of terpenes as possible. I've found lab results showing thca will naturally decarb in tincture within four months to as much as 87% efficiency. Unfortunately, terpene levels were not analyzed. I'm excited to be able to tag along with this thread as some of the mysteries of terpenes unfold. At this point, my biggest unknown is degradation rate of terpenes extracted in ethanol. According to your find, it appears degradation in raw plant matter results much quicker than I had imagined leading me to possibly start my natural decarb tincture immediately after harvest. Been here only a day and already gleaning useful information. Thanx

 

[Canyon]

Interesting article, oldbear. Thanx. I've been making ethanol tinctures for the past year. Irrelevant of the strain I use, I'm getting more of a sedative experience than I would prefer. I understand the personality of cannabis is due to the terpenes so I'm on a quest to create a tincture while maintaining the highest level of terpenes as possible. I've found lab results showing thca will naturally decarb in tincture within four months to as much as 87% efficiency. Unfortunately, terpene levels were not analyzed. I'm excited to be able to tag along with this thread as some of the mysteries of terpenes unfold. At this point, my biggest unknown is degradation rate of terpenes extracted in ethanol. According to your find, it appears degradation in raw plant matter results much quicker than I had imagined leading me to possibly start my natural decarb tincture immediately after harvest. Been here only a day and already gleaning useful information. Thanx

If you use the frozen quick wash method and either reduce the alcohol content to the concentration you want or remove all the alcohol and add whatever you want to dilute it with, I don't think you are going to lose a lot of terpenes in the extraction process itself. With a 120 day decarb the effects of aging would probably increase even sealed up. The terpenes should be better retained without the heat and sealed. The problem I see is,the loss in the drying. Four months at room temperature would have me concerned about it going rancid.

I have played around with rosin when I have had extra material. For me, I get inconsistent results and yield.What I have noticed is with the more moist buds and lower temperatures I get a nice sap like oil compared to shatter like results of higher temps and drier buds. There is something going on there and I suspect retained terpenes are a big part of the difference.

OB, Sue, do you think adding oil only to FH buds and doing an extended pressure cooker infusion/decarb would work? I have visions of an oily mess to clean up.

kickn, Bag seed plant is special, though not an heirloom. I saw it on a coffee table and on a whim I stuck it in my shirt pocket while I was visiting in Ca. I have been growing it for nearly five years now. I actually have a smallish one in early flower now.

 

[Canyon]

Bucudinkydow,
With alcohol going rancid would not be a problem. With oil it could be.

I never know

 

[SweetSue]

Nothing says science like storing in a brown paper bag waiting for the majick to happen. lol Right beside the banana ripening study.

Hey..... I'll have you know my finish flowering tent has never produced the buds it has since I started keeping a bunch of ripening bananas in there. Not only does it supply me with a delicious wake-up snack, it's works to increase yield. I'm living proof that it works.

Sometimes stoner science pays off big time.

 

[SweetSue]

If you use the frozen quick wash method and either reduce the alcohol content to the concentration you want or remove all the alcohol and add whatever you want to dilute it with, I don't think you are going to lose a lot of terpenes in the extraction process itself. With a 120 day decarb the effects of aging would probably increase even sealed up. The terpenes should be better retained without the heat and sealed. The problem I see is,the loss in the drying. Four months at room temperature would have me concerned about it going rancid.

I have played around with rosin when I have had extra material. For me, I get inconsistent results and yield.What I have noticed is with the more moist buds and lower temperatures I get a nice sap like oil compared to shatter like results of higher temps and drier buds. There is something going on there and I suspect retained terpenes are a big part of the difference.

OB, Sue, do you think adding oil only to FH buds and doing an extended pressure cooker infusion/decarb would work? I have visions of an oily mess to clean up.

kickn, Bag seed plant is special, though not an heirloom. I saw it on a coffee table and on a whim I stuck it in my shirt pocket while I was visiting in Ca. I have been growing it for nearly five years now. I actually have a smallish one in early flower now.

When I read the original post my first thought was to make a batch of FHO instead. It can be used in the same way as a tincture, although it won't absorb quite as quickly as the alcohol-based tincture would. But the medicinal effects would be so superior it'd be worth exploring.

Bucudinkydow, is it necessary that your administration method be a tincture?

Incidentally, it's recommended you store THCa products in the refrigerator to slow down that conversion rate.