So, I work in a reputable, legal lab in MO and about three months ago, our state regulations made it mandatory to test all concentrates for vitamin E. At the time, it seemed like a joke; I figured that at the very least we’ll be able to know if people are being shady…flash forward to now, and I’ve had four SHATTER samples come back for extremely low levels of vitamin e acetate (.049ppm,.014ppm,.086ppm, ect). I’m very perplexed at how this has infiltrated our lab and im trying to get to the bottom of this.
I have a couple theories:
1.) The analytics we’re receiving from our testing facility are skewed/ tainted in some manner (false positive?).
2.) Some sort of conversion of terpenes/volatiles, cannabinoids.
3.) Cross contamination; but from what? we have not changed our practices for creating any of these sku’s, I feel it would have presented itself in a bigger manner if it’s being cross contaminated. I’ve only found it like I said in CURED flower extracts, never any fresh frozen/ live.
4.) one of my employees really likes vitamin e and is tossing it into our concoction when no one is looking. (this is a joke, I hope) lol
Cross contamination can come from seriously anywhere. With limited amounts needed and the substance showing up in weird places semi-often… it could also be that people upstream of you were using it and haven’t actually replaced or sufficiently cleaned. I see that A LOT for pesticide contamination, no reason that it wouldn’t happen with this difficult to “clean” substance as well.
Combine that with what @TheVanillaGorilla said - and consider that MANY not all but so many sunscreens have this in them and aftercare stuff. People started going outside in Missouri in the last few months - its been fucking hot and there’s plenty of fun to be had in the sun.
So yeah - you might look at cross-contamination. And you might also just ask your supplier similar issues can happen when people are harvesting and plants get contaminated.
The limit is low enough to be incidental. So if people are exposing their skin to the plant at any point, you could have enough incidental that is getting concentrated to be noticed on a sample.
I always question results of new tests until I see their method validation data - if you don’t already know the answers to their questions. You should. You have someone supplying Final Product Testing for you - you or someone at your company should have an intimate understanding of their operation AND their laboratory investigation process for looking at OUT OF TREND issues just like this.
If the lab isn’t interested in working with you on this - look for a different lab. They should be its part of their certification process.
If you need help on this. HMU in the DMs. I don’t mind poking around labs and asking the questions to get to the answers that are needed. And I also support folks in going back to regulators and asking them to make rule changes, etc.
From that it looks like they think they have things validated well. You should still ask them for a lab investigation. And also ask them if they are having other failures happening around the same time as yours.
Its possible their LC column is contaminated from someone else and they didn’t run enough flush/blanks to fix it. You know?
Every other bracket, it declares how they test, but for vitamin e, its undeclared. ill contact our testing agency we use and ask them. I’ve been wondering how they’re testing for it as well. I appreciate the responses. makes me feel less crazy.
I’ll update if I find anything worth mentioning.
PS. it seems as though, for what it’s worth all testing agencies are kind of suspect, in just my honest opinion, from calibrating machines, new employees, accidents on their end.
I remember a couple years back i was getting three badders tested, they fucked up on their end and switched one batches terps for another…I just noticed due to the intrinsic nature of cannabis to me, I knew that certain terps where not present. people at my company thought I was being nitpicky…turns out I was right and the tech at their lab found his mistake, then they apologized. our testing company we work with is pretty tight with our owners as well so that adds complexities.
I just genuinely want to find solutions to deepen my understanding of all things in our world, and sometimes that’s easier said than done.
Tocopherols are native to plant tissue. I wonder if they are finding some other tocopherols or tocopherol-like compounds that elute at a similar time. Mass spec might help followed by NMR
Bro I think nowadays if you purposely put vitamin e into your vape carts you should go to prison. And I mean more than just a few parts per billion. I mean if you add some in.
Nothing more that two orders of magnitude. Some things at only 50% of action level…
Sigma lists an hplc method that they claim can be used on cannabinoids and vit e with the same injection. Not sure it could manage an appropriate LOQ for your regs while also giving decent quantification on thca in the products you’re testing.
That should make asking the hard questions easier…
ICH practice for this would be like 3 degrees of magnitude below - or 0.005. Leaving it at 0.001 would mean you were not having to do weird things from reference standards (which are often, but not always 100, 10, 1, etc).
That’s why he should look at the validation documents - or ask the questions.
They are probably running on a LC some people run this test at the same time as say pesticides. So a prepped standard and control samples would be quite dilute on the calibration curve.
And I agree:
And if it doesn’t - well then you know that the issue is inappropriate business practices and should look to be somewhere else so that data fraud and other such issues don’t come at you and land you in a world of hurt.
We’ve had similar issues with testing labs in MO. It’s a crap shoot out here sometimes man.
We’ve seen the vitamin E acetate pop up in distillate… seen benzene randomly pop up in badder (tested our gas with a 3rd party and no trace of benzene). I guess it could’ve been related to terp degradation but I’m not sure how, when we never heat it over 100F.
Seen acetonitrile in samples, which is commonly used in testing labs but we don’t even have it on site.
This is why you’re not allowed to wear medicines, cosmetics, jewelry, scents, or other similar products into clean room drug manufacturing suites. If you can smell it, it is in the air and falling everywhere. If it is on your body, when you put your arms and hands over open containers, your human dander is falling into it. Aseptic technique makes this less of a problem (no extremities or face over open containers).
We had an event where someone wearing a ton of perfume walked into a flavoring suite while carts were being made and it failed for all sorts of crazy, including benzene.
