Lab Failure? Or My Failure?

decarboxylation
testing
ethanol
#1

So i just had a batch of RSO syringes fail Phase III (California) compliance testing for residual solvents. (Ethanol and Acetonitrile) it didn’t make sense to me, but maybe i might be overlooking something? Here are the lab results: (GC/FID w/ Headspace Analyzer)

I had to look up what Acetonitrile is, because we don’t use it in our lab. After doing a little research, i discovered that it’s a commonly used solvent in gas chromatography? Just so happens that all of the residual solvents that were detected on that test are used in gas chromatography. Coincidence? Hmm…

Now let’s address the ethanol. I’ve been utilizing the Gemstone decarb SOP with great success up to now. Every batch passed all compliance testing with flying colors this whole year. I’ve been decarbing over a hotplate stirrer for an hour at 130c. Now i was under the impression that my temps won’t exceed 80-90c until all the ethanol has been purged. Is it even possible to have any residual ethanol remaining in a fully decarbed solution? The only thing i could think of is that i did have a fan blowing towards the decarb station to keep the vapors moving as they boil off. Is it possible that the cooling action of the fan blowing on the surface might’ve prevented the ethanol from evaporating? This was a 710 ethanol extraction of 10 lbs of starting material extracted with a CUP15, ending up with about 700mL in a 2L glass beaker.

It’s worth noting that we did do an R&D test (from a different lab), and it came back with ethanol levels ND. This lab was using GC-MS.

Please correct me if I’m wrong, but am i mistaken for thinking that mass spectrometry is better suited for ethanol detection over flame ionization detection?

So here’s the fun part. Here in California, all testing labs automatically report test failures to the BCC so now we have to submit a corrective action plan, and then request permission to remediate this batch to resubmit for testing. Fun times! Have any of my fellow licensed manufacturers in California had to deal with this yet? Not sure we can even go with another lab at this point to retest. The law is setup to prevent us from shopping labs once a sample has been taken, but without any quality assurance standards to hold these labs accountable, what option do we have if the lab is causing us to fail? Any insights or some perspective would be sincerely appreciated. Thanks in advance!

6 Likes
#2

Call the lab and bitch them out.

4 Likes
#3

It does seem like lab error. They ought to be open to doing a re-preparation and retesting at the same lab, which is not shopping. Just ask and explain these concerns to them.

5 Likes
#4

What about your methanol, isopropanol and ethyl acetate levels?

#5

Every time one of our samples has failed it has been a lab testing error

2 Likes
#6

Maybe I read that wrong, but are you using denatured ethanol for RSO?

Maybe the lab is wrong, but maybe you are introducing non-food grade solvents with traces of toxics into a food product?

#7

Where do you buy your solvent? I assume when you said “710” that you were talking about 710 Spirits, which is 95% ethanol 5% heptane, correct?

It would be worth testing your solvent. Check this spec sheet out, for example:

1 Like
#8

If this is the only solvent you’ve introduced and you have a GC-MS result of the same material as Ethanol-ND, it seems likely that the lab has made an error (perhaps contamination with another product that was high in ethanol?)

At any rate, call them and tell them to retest it. If the next etoh reading is a few standard devs out of the range of the first, they fucked up

1 Like
#9

Have the Lab re test. The one time we failed CAT lll the Lab re tested and found it to be an error on their part. I even received a call from the owner as he found it very strange that we failed.

4 Likes
#10

There’s no reason for acetonitrile to be in your solvent. Heptane yes, methanol, maybe. But this looked like someone has a Quechers extraction carryover problem in their analysis. But what do I know? I’m only an analytical chemist who specializes in ms and volatile methodologies
Retest…it won’t be there

8 Likes
#11

@Soulboy I work at SRI Instruments. Which lab is this? Why are they using 2ug/g? It looks like the math is incorrect.

#12

@Soulboy Myself or an SRI technician could give them a call if you like, and see what’s going on with their technique, calibration, etc.
Potentially it could be a win win. The lab may be grateful for you saving them embarrassment & future unhappy customers, and you yourself, could get your well deserved answers and or your money back.

Summer
SRI Instruments

5 Likes
#13

Thats a prime example why you should always do your compliance testing with the same lab that you did R&D testing with. I noticed you used PH Solutions for the test sample. you should just stick with them, they are the best lab in the state in my opinion

1 Like
#15

Thanks for the responses, everybody.

In regards to the concerns about 710. The 710 is made with food-grade ethanol. The heptane as you can see from the test results posted, is not present in the final product. The solvent is not the issue, as batches upon batches of products made from it has passed compliance testing before and after this one.

Our operations manager has been handling all the correspondence with the lab. It seems that they are pot committed, and are insisting that all lab protocols are being followed, and that it’s not an error on their end. Not that there was really anything they could remedy, because the damage is done. Once the COA is issued, it can’t be amended, nor can it be retested.

I think the best i could hope for is to submit remediation plans to the Bureau and then request approval for retesting by a new lab on grounds of the initial lab being unable to competently complete testing, but even that seems to be a longshot, because this request is supposed to be made before the COA was issued.

We’ll see how this plays out. Its moments like this that make me realize that we need to start showing up at those BCC hearings and start joining the conversation and speak out, because if we don’t, nobody will do it on our behalf.

So yea, moral of the story…don’t cheap out on your lab testing, and do your due diligence and vet your labs! Find out their methodologies and ask questions on how they handle disputes or disagreements on bad test results! If they’re offering crazy discounted deals and incentives, there’s probably a reason why. Learn from our mistake!

As for which lab this was, i don’t want to name names and draw unnecessary attention by way of a Google keyword, but let’s just say that their name rhymes with Charm Dabs. : ]

Thanks everyone!

1 Like
#16

No reason you can’t post the name of the Lab for the rest of us. I would send another sample to a different lab. It should get a pass and then you can present your case to the bcc. This is the reason we spend the extra $$$ and do R&D tests first.

4 Likes
#17

That’s what I’m trying to tell you guys. The laws in California are setup in a way that doesn’t allow you to just retest. The lab that issued the COA is not allowed to retest, nor can they amend it. If a lab fails you, it gets reported to the Bureau of Cannabis Control, and then the product must be quarantined. It has to either be destroyed, or in some limited cases you can request to remediate the batch. This is only allowed for labeling discrepancies, residual solvent failures, or when certain pesticide levels are over acceptable limits. You have to submit an action plan, and then you’re at the mercy of the Bureau. But the retest has to be done by the same lab. They don’t want manufacturers to be able to shop labs until they find the one that will give them favorable results. This is my frustration with the way it’s setup. If the lab is the one responsible for the initial fail, then no amount of remediation will fix the problem. And since the law prevents me from getting it retested, there is no way for me to establish that there is nothing wrong with the batch in the first place. All of this is an incredible burden on manufacturers, who are paying $600-$800 per test, if they are lucky enough to remediate. Otherwise we would have to destroy the product, all because of an incompetent lab.

#18

It’s called an R&D test my bro what you should be doing. These do not get reported to the state. You need to find a new Lab asap. The one time I failed an R&D test I was called to let me know they where going to retest the sample to be sure. Like I said find a new Lab and establish a relationship. Talk to the #1 person at the location and ask for a walk thru. If they don’t want to let you come by go elsewhere.

2 Likes
#19

Always test before official COA. That’s my stance. Bring it in-house if you can, if not, pay to test for your “watchouts” before COA. But none of this really helps you in this case.:pensive: But BG305 is right. Find a lab thats willing to R&D test for you. Would be awesome if they can also COA for you after. I stand by my theory that this is simply carryover from a pesticide extraction previously on the instrument. Or simple contamination (the acetone numbers). Either way, dump them in a hurry. Especially if they didn’t try to communicate the gross outages they saw in their analysis prior to official posting of the COA. This kinda screams incompetence in my opinion. You probably got the new technician …just sayin

2 Likes
#20

Wow, that law is much harsher than Oregon’s. Oregon at least allows retests (from the same lab, no shopping), which is totally reasonable. They are putting a lot of faith in the lab results being correct every single time but even the best labs will eventually make a mistake. Even an r&d result won’t stop it because a lab could still make a mistake in the final COA and get locked into it.

2 Likes
#21

@Mattman Agreed. What kind of in-house testing are you working with?