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Comment · Sat, May 18, 2024 · ND Owner

u/MisterYouAreSoDumb asked me to post the Lab Testing COAs I received from Bulk Supplements (Below)

What they were answering

Direct reply to the original post in this thread.

u/MisterYouAreSoDumb · ND Owner

That's about what I expected. These are just internal COAs. To start, analyzing nitrogen content is not an appropriate methodology for amino acid assay. This is the same shit China got away with on infant formula and spiking melamine. They used melamine to fool the nitrogen testing to make the protein content seem higher. The basic testing for protein was a simple nitrogen assay, which the Chinese figured out you could trick by putting melamine in the formula. This would make everything come out okay, because the testing was only looking at the nitrogens. Well a shitload of things have nitrogen in them. That assay could be showing anything with nitrogen in it and it wouldn't know the difference. Could be L-carnitine. Could be melamine or another amino acid. The methodology wouldn't know the difference.

So why do people use nitrogen analysis for amino acids? Well, it's the lazy way. Most amino acids don't have a chromophore. This means that the UV detectors in HLPC or UPLC machines can't see them. So what do you do if your machine detector is blind to the molecule you are trying to analyze? It's called pre-column derivatization. This is where you take the sample you are analyzing and react it with something that will attach a chromophore to the sample. Then you can see the chromophore of the attached moiety, and assay the analyte that way. I will give you a few examples of some amino acids.

Here's an assay of L-carnosine that we passed.

That's a UPLC test using Waters' amino acid kid that uses pre-column derivatization. You can see four peaks there. The first is the AMQ peak, which is the reagent peak from the Waters sample prep. Peak two is ammonia. Peak three is the carnosine. Peak four is the derivative peak. You then inject a standard solution of L-carnosine from somewhere like Sigma Aldrich, and you compare the area of that peak to the area of the carnosine peak in your run. Then you calculate the purity. That's the appropriate way to assay amino acids. If you want to read more about pre-column derivatization assays for amino acids, you can read more about it on Waters' site.

https://www.waters.com/nextgen/us/en/education/primers/comprehensive-guide-to-hydrolysis-and-analysis-of-amino-acids/derivatization-of-amino-acids-using-waters-accqtag-chemistry.html

I'll share a few more as examples.

Here is an L-arginine assay.

Here is a batch of L-arginine we failed.

Here is an L-arginine assay of a finished capsule.

Here is an assay of L-tryptophan.

Here is an assay of a batch of L-tryptophan that we failed.

If we just tested for nitrogen content, we would have no idea where the nitrogen was coming from. It's just a cheap and lazy way to test amino acids that is rife with adulteration from China. They know how to beat these nitrogen assays, which is why you need better methodologies. This especially goes for protein powders. We have done some analysis of popular protein powders on the market, and the amount out there that are just spike with cheap nitrogen sources would astound you! You need full amino acid analysis to really tell quality.

The other issue I have is the fill weight "test." The average fill weight being exactly 500mg is odd. I can tell you right now it is NEVER exactly what your spec is. Literally never have we had our average fill weight exactly spec. It's not how manufacturing works. Your machines always have a manufacturing tolerance that you account for. We always account for a 5% manufacturing tolerance, and then buffer for things like NLT assay specs and water content.. I'll give you an example.

Here is our worksheet calculation for a recent batch of lion's mane 1:1.

Ours Lion's Mane 1:1 capsules are 500mg each. There are no fillers. You can see that we always buffer up, so that nobody is ever short for any reason. Literally no other brand does this. We account for all worst case scenario tolerances into our systems, because I just know if I let one capsule out one time that is short, some Jabroni is going to call me out on it. That, and I value always having what you claim on the label. We do gross mass and fill weight mass. Gross includes the weight of the capsule. The capsules range in mass as well, so you have to weigh the contents along with the gross. Mean average fill weight for this batch is 524.525mg. You will never ever see a COA from us saying a spec of 500mg with a result of 500mg. It's just not going to happen. Statistically it's impossible. When I see a result like that, I know this is a "by input" COA, or the stupid scam that going around right now where people just review MBRs, or master batch records, and say: "Yep, they say they put 500mg in there, and that's what this MBR says, so good enough for us! It has 500mg!" Even Eurofins is doing it now. It's insanity! We have been screaming at Amazon to stop allowing this practice, but for some reason they keep allowing it. Unless you assay a finished capsule, like I showed above for some of those UPLC results, you have no idea if what you say is in there is actually in there. This is especially true if you have to use any fillers or excipients. In our lion's mane 1:1 we didn't, so our mass testing was easy. However, that is not the norm. Most of the time you have to blend your powder with other things to help them flow in the machines. If you just trust the MBR, or only rely on mass testing, then you have no idea if your formulation was done right. I can tell you right now that sometimes formulation is a pain in the ass. Some things mix well and flow well. Other things are a nightmare. We do in-process assaying to ensure our formulation is correct before moving on to full production. Almost nobody else does that. It results in a lot of headaches, let me tell you. We've been trying to get DHEA quick dissolve tablets out for a while now, but the in-process assaying keeps coming in low. Such a pain in the ass, but it's what everyone expects of us. If you buy DHEA from us and it only has 4.65mg in the tablets instead of 5mg, then I have failed you. So we do what is needed to ensure it is right before it gets out to all of you.

Anyway, now I am ranting about details most of you don't care about. We've tested a bunch of stuff from Bulk Supplements over the years that has failed our testing. Because of those results, I just don't trust them at all. I have not tested anything in the past year or so, though; so I will have to pick some things out and run another round to see how they are doing lately. I am just fairly jaded from years of failing test results, even from brands I used to trust, so these days I am mostly a cynical asshole. Ohh well, that's my role now. I am the cynical asshole of the industry. I will just own it.

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