Variance in d8 lab results: An analytical review

[bigbone]

@kcalabs

The coelution on the HPLC isn’t because d8 and d9 aren’t resolved.

The peak distortion is caused by coelution of other substances that are produced during the synthesis of d8-THC

I understand this, but which compound are you overestimating in this coelution of multiple isomers considering only two compounds (D8&D9) are integrated on the HPLC method?

@Mcfly

The results from @kcalabs were perfectly within the average and standard deviation justifying their crown.

@eyeworm

everyone be dick riding without proper justification or without criticism of a flawed method

I think this is my biggest problem. I do appreciate your activity and transparency in regard to most issues raised. However, there are other labs that use GC separation to convince customers that the D9 they are reporting from their HPLC is actually present since there is clear baseline resolution on the GC. Yes, you are very active in this community, but that alone shouldn’t give you the gold stamp of approval. I don’t criticize to harm people or businesses. I criticize because the science needs to be improved.
An outside proficiency test on your GC method would be a good start. Including it in your ISO scope would be the way to go, but I 100% understand not wanting to keep throwing money at the hungry ISO accreditation dogs that are really not doing anything to improve the science. Yes, traceability is very important, which is the only thing I consider if I see a lab is ISO accredited. It speaks nothing to their methodology, which is a shame and what people need to understand.

[kcalabs]

@bigbone

I understand this, but which compound are you overestimating in this coelution of multiple isomers considering only two compounds (D8&D9) are integrated on the HPLC method?

The methods we are using to determine d8-THC and d9-THC are accurate and precise.

@bigbone

Yes, you are very active in this community, but that alone shouldn’t give you the gold stamp of approval.

I’m not sure why this is our problem? I’m not asking for anyone’s gold stamp of approval. If you’re upset about this then raise it with the community and convince them otherwise.

@bigbone

I criticize because the science needs to be improved.

The science does need to be approved and I would argue that we are on the right side of the fence on this topic.

@bigbone

However, there are other labs that use GC separation to convince customers that the D9 they are reporting from their HPLC is actually present since there is clear baseline resolution on the GC.

If there is no clear baseline resolution on a HPLC method, then the next step is to conduct more experiments to try and resolve them. This has led to a better understanding about what is interfering with d9 and d8 and why HPLC has flaws when testing these products.

[Kingofthekush420]

@bigbone

I think this is my biggest problem. I do appreciate your activity and transparency in regard to most issues raised. However, there are other labs that use GC separation to convince customers that the D9 they are reporting from their HPLC is actually present since there is clear baseline resolution on the GC. Yes, you are very active in this community, but that alone shouldn’t give you the gold stamp of approval. I don’t criticize to harm people or businesses.

I’m just curious

How many cannabinoids does your method test for on hplc? @bigbone

@kcalabs don’t you test for 22 plus the internal standard?

[thesk8nmidget]

@kcalabs

If there is no clear baseline resolution on a HPLC method, then the next step is to conduct more experiments to try and resolve them. This has led to a better understanding about what is interfering with d9 and d8 and why HPLC has flaws when testing these products.

Is there a reason you have to include the HPLC graph and not the one showing the baseline separation? or better yet both graphs and or a little note that clearly states something like: “This was not the only method or chromatogram used to quantify these results.”

Anyone reading that COA would and should assume that the graph posted on the COA is the graph you quantified your results from and should be concerned with the lack of separation.

[kcalabs]

It is our SOP, so that is what we follow.

We’re in the process of getting that changed, finalizing development of our new software, and we’ll have a new COA coming out soon.

This won’t be an issue soon.

[thesk8nmidget]

Perfect!

I personally know you are using secondary methods to verify but I also can see how misleading it could be to someone that doesn’t know your procedure.

[bigbone]

I am a researcher that doesn’t need high throughput on samples, so run time isn’t an issue for me when making an HPLC method to cover all the cannabinoids there are standards for. Although, I only use HPLC when interested in acidic cannabinoids. GC is my go to instrument for analysis.

[THCA_Synthase]

Is this to say that KCA runs two methods on every potency sample, one reverse- and one normal-phase? That would be very expensive.

My internal lab has found KCA to be pretty distorted compared to recreational labs we have contact with back west. Hemp laboratories benefit from much less oversight than labs in established rec markets. KCA likes to read old literature and to assert things they have not proven, much much too frivolously.

[pdxcanna]

sounds like you have some data to put forward to support your claim then?

[moveweight]

I see a lot of newcomers with a lot of talk.
How about we have a competition on who’s the best testing lab while we also chase compliant d8.

Because nobody else seems to walk the talk around here outside of maybe a few testing labs on here.

How about you naysayers get off your armchairs and put some validity to your statements.

Thc testing labs have far less hassle and less oversight. Your generalization sounds based on your experience. Come to Oklahoma and tell me a thc testing lab with more oversight than a DEA registered lab testing samples from all across the country…

“My internal lab” reads like “my in-house testing” btw.

[Dr_Jebril]

@THCA_Synthase

My internal lab has found KCA to be pretty distorted compared to recreational labs we have contact with back west.

Well… you could be all distorded.

Based on many discussions here, with data, not only dealing with d8, many rec labs are quite distorded.

[kcalabs]

We run the distillates on two instruments to ensure we get separation between the isomers present.

Distorted how? We’re a hemp lab, which means we’re much more interested in the low end compared to rec labs.

We read old literature and assert things we have not proven? I guess Mechoulam is considered irrelevant to you?

Happy to have a conversation about why our results differ, but our team has been in the testing industry for decades.

[kcalabs]

@Kingofthekush420, 18 accredited plus internal marker and then another 6 that get run routinely as part of method validation work.

[kcalabs]

Happy to compare data. If @THCA_Synthase wants to let me know who he/she is and gives me permission to share data we can put it all out there.

If we’re proven incorrect I’ll start a CAPA and bring it up to the team for continuous improvement.

[Kenley]

Have you guys had any tests come back d9 compliant yet?

[kcalabs]

Yes, two actually. @lady420

[THCA_Synthase]

You are incorrect. The strictures are just new to OK, but not in previously legalized states.

As a generalization, recreational testing laboratories suffer much greater oversight right now than national hemp laboratories do. In my experience, there is no effective policing of analytical laboratories under the Farm Bill.

I get why these assertions would provoke a defensive reaction in analytical groups. I am admittedly blunt, and I apologize. It’s a very, very difficult business running a commercial laboratory, it is nearly impossible to both run good analysis and turn a profit in a mature market.

[THCA_Synthase]

Of course Mechoulam is not irrelevant to me, but I didn’t mention him. He is a niche and respectable chemist! I find–observing your responses to others–that you draw a lot of facile connections with things in the literature that strike me as frequently unsubstantiated and in error.

Our results will definitely differ, that’s always the case? A client running analysis in a new locale needs to understand their results within the testing environment around them. We run ring tests on a variety of samples for them to better understand the meaning of their results to THEIR clients.

Western recreational states under much stricter oversight tend to coincide with my methods, because I have calibrated them as such for MY accuracy. Hemp laboratories operating predominantly west of Colorado, tend ti disagree with our established methods, and with trusted entities with a long track record.

[moveweight]

I call bullshit

Take me to thc testing labs in Oregon, Colorado, Ohio, California, Nevada that have more oversight than a DEA registered testing lab. I’ll afford the plane ticket and give you a pat on the back. Just because I used Oklahoma as a reference doesn’t mean it isn’t so for other states as well.

Blunt but without validity to your statements…

Best joke all night

@THCA_Synthase

Western recreational states under much stricter oversight

West coast oversight. GTFO of here lol
Now I know you’re not from the industry.

I needed a good late night laugh. Thanks…
If I had a dollar from every shitty coa on the west coast.

Or a dollar for every thc testing lab that can’t get d8 right lol isomerization products invaded rec too

They still think d8 is compliant mostly

@THCA_Synthase

It’s a very, very difficult business running a commercial laboratory, it is nearly impossible to both run good analysis and turn a profit in a mature market.

Here’s the truth. $$$$ Good testing labs are being out moneyed by shitty ones. 40% flowers sell better than 14%. Compliant d8 sells better than hot d8.

Meanwhile Doug Varin is supposed to have d9thcv

Someone wanna go test this and tell me it’s got no d8thcv? Because I’m at the stage of betting money this recreational product is isomerized and sold as natural.

They claim their strain has d9thcv. Of which I believe. I however know they’re subsidizing d9thcv with d8 in a rec environment for vaporizers and other products. Why? The answer is simple. $

Crave away product is pure d8thcv.
So here they state their cbn sleep has d8thc, but what do you think their thcv advertised products without the d8 in the ad… have? Go test and report back I wanna see 30% d9thcv vape results.

You mean to tell me this has more oversight? Because I don’t believe it. Dudes selling hemp at above Cali weed prices lol (prove me wrong please I hope you do) because I’d like some d9thcv concentrate I can trust and their obvious involvement with Isomerized products has me believing they’re backdooring d8thcv also as their THCV line of products. 3% thcv pre rolls… You’d think they’d pump out flower… But they list CBDv and CBG and THCV as what they grow. Hmmm. Idk fam. I’m seeing a hemp outlet with a thc license playing the game hard.

Marin County and Bay Area Weed Delivery — ONA.Life

This competitors product however I want to definitely try. But then again SC Labs…? That one rings a bell too. Idk if good or bad. Just remembered reading about them. Shady Lab Results

[bigbone]

@moveweight

DEA registered testing lab

FYI. DEA doesn’t even look at your methods during the registration process. They check your security and sample disposal.