6 replies to this topic

[Brothbro]

Hi All,

 

I'm with a small dietary supplement manufacturer, making herbal supplements in the form of capsules, tinctures, and loose powders. Some of our products are blended, meaning we'll mix powdered herbs together based on a recipe (eg 50% Gingko 50% Gotu Kola). Some of our blended products have 5 or 6 different herbs mixed in different proportions. We're currently working through some labeling/composition testing compliance issues. 

 

Our specification sheets and product "supplement facts" panel list that each capsule or serving contains a certain mg content of each ingredient. Currently, we arrived at this mg content through the "by input" method. This means that the mg content of each herb in the blend is not tested for after blending, rather it's calculated based on the ratio of ingredients in the bulk batch. For example, if 100lbs of Ginkgo Gotu Kola blend (50lbs of each herb) was encapsulated, each 500mg capsule is assumed to contain 250mg each of Ginkgo and Gotu Kola powder. This of course assumes that blending is homogenous. The FDA has been coming down on supplement companies over the past ~10 years about composition "by input", they would rather testing be done on the capsules themselves to quantify the actual mg content of each constituent.

 

This is where the problem starts: I can't seem to find any testing labs that can quantify the amount of herb in a blend. Detection (presence/absence) is easy enough, but that doesn't go far enough to actually very that the capsule contains what the label says it does. If these were vitamins they would be quantifiable through testing. But our ingredients are simply freeze-dried herbs milled into powder. 

 

The best testing option that I've come across with a lab is to create an HPTLC reference profile for each of our blends to which subsequent lots can be compared to. So sure, we can send batches along as see that the HPTLC banding matches up, but how does this relate to mg content of each herb? We'd like to establish a spec range of mg content for each herbal constituent in the blend. How would we be able to tell if we were only slightly off on our herb blend based on HPTLC data? I doubt we'd be able to.

 

I'm almost considering filing for some kind of exemption with the FDA, based on the lack of scientifically valid methods for verifying the mg content of each herbal ingredient. But we're certainly not the only herbal supplement company out there, so a solution to this must exist. Anyone else in the herbal supplement business have any insight into this problem? Thank you for taking the time to read this long post!

[Rhewitt33]

Brothbro,

I worked for a Nutritional Supplement Manufacturer years ago. We used Eurofins to get the quantitative testing completed. I would pick an ingredient out of, lets say 6, and ask for amount found in 20 capsules or so. I cannot remember the amount in weight we had to send. About a week later, Boom. Results. I know it was pricy and I don't even know if they still do it. But that's who we went through. 

Hope it helps 

[Brothbro]

Thanks Rhewitt33,

 

I've reached out to Eurofins to see if they have this testing capability! Did you work with herbal supplements specifically? I think the availability of quantitative tests may hinge greatly on the ingredient tested for. Quantities of Vitamin C or Quercetin can be easy to measure, while mg of nettle leaf may be more difficult...

 

I do know that for some herbs a "marker compound" is selected, which can be quantified. For example, curcuminoids in Turmeric. But these marker compounds vary naturally with growing conditions, so it doesn't seem practical to use them as an indicator of how many mg of Turmeric powder there is in your blend.

[AltonBrownFanClub]

What about using known values of micronutrients to calculate it?

 

For example, say one capsule should contain a 50/50 mix of Gingko and Gotu Kola.

 

You use Ginko's known value of 50mg Vitamin C per 100g.

You use Gotu Kola's known value of 100mg Vitamin C per 100g.

The resulting mix should have 75mg of Vitamin C per 100g.

 

Now lets say your finished products tests at 99.5mg of Vitamin C per 100g.

This would mean it is 99% Gotu Kola and 1% Ginko. You could make a graph plotting all test values.

 

Not feasible for products with many ingredients, but would possibly work to validate a process.

[Evans X.]

Greetings, 

 

I agree with the process in post #3 but with a small correction. Since you don't know the exact chemistry that takes place during the blending and how can elements from one or the other be lost the 99.5mg could be translated in a range of 1% to 25% gingko (meaning you could get 75mg vit. C from gotu cola and 25 mg from gingko).

As herbs contain multiple "ingredients" your best option could be to determine which of these are the necessary ones that you advertise as supplementing the diet and work with them. Test raw materials for these (eg vitamins, trace elements etc) and then test end products to see if you get the expected values through the blending, like in the example in post #3 with the 75mg vit. C result.

This way you can also indirectly conclude that you get 250mg from each herb in the 500mg capsule, more so if you can back it up for a few specific substances. In my opinion don't go testing for heavily difficult/specific-to-the-herb substances, it can be more valuable to choose a wider range of easier to trace elements and propably less costly.

 

Regards.

[Brothbro]

Thanks AltonBrownFanClub and Evans X, I do think some kind of blending process validation may be a good route to take based on micronutrient content from quantifiable sources. I'm considering doing a validation project on the blending process itself, to establish blending time as a process control for composition. Perhaps by mixing vitamin blends (or any other quantifiable substance of similar physical characteristics to herbal powders) in the same proportions as our herbal formulas, we can validate through testing that the blending does result in a finished product with each ingredient in the expected percentages.

 

Rhewitt33 - I did reach out to Eurofins, and unfortunately they are unable to do composition testing on our product. Since we do not standardize our products to a certain content level of "active" ingredient, quantitative testing is not reliable because the levels of these "active" ingredients vary so much between harvests. Our company's focus is instead to provide herbs as close to their natural state as possible. For example, through freeze-drying we preserve milk thistle to produce a higher quality product than an air-dried counterpart. However, we are not making any claims as to the Silymarin content of the milk thistle, which is an antioxidant that generates most of the customer interest in the herb in the first place. Our label simply claims the mg of milk thistle powder per capsule, where as other brands might also state a certain ng content of Silymarin. Silymarin is a quantifiable substance, while Milk thistle in general is not.

Edited by Brothbro, 05 May 2022 - 06:28 PM.

[Scampi]

I think HPLC may be the way to go

 

When I was in cannabis, that is what we were using to determine the amount of THC or CBC in a solution

 

We had a declaration of potency of the input, but HPLC was the only was to identify finished solution concentration across a batch