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Confused about Raw Material identification Requirements?

Confused about Raw Material identification Requirements?

I understand there is still a great deal of confusion surrounding the Raw Material Identification requirements in the Dietary Supplement GMP’s. I hear from clients daily that they still don’t know what to do, how to do it, and when to do it. Let’s see if we can help clear up some of the questions folks are having out there!

First off, let’s review the regulations so we know why ID testing is required. According to 21 CFR Part 111, Subpart E, 111.75, “before you use a component, you must conduct at least one appropriate test or examination to verify the identity of any component that is a dietary ingredient” What that means is that for every unique lot of incoming dietary supplement ingredients, you will need to conduct at least one test or examination that will confirm the identity of that material before use approve it for use and use it in manufacturing.

Let’s be clear about the unique lot of incoming components before we move on. Let’s say you receive a shipment of Vitamin C. You ordered 500 kilograms of Vitamin C and the shipment arrives at your dock. When you do your receiving inspection, you have 2 50 kilo boxes of lot#A360, 4 50 kilo boxes of lot#B720, and 4 50 kilo boxes of lot#A470. To comply with the regulations, you would need to conduct your identity test of a sample from lots A360, B720, and A470, so you would need to do three identity tests on this incoming shipment because it contains three different lots of material, even though it’s the same material, received at the same time. Its always a good idea to request that your order be filled with one lot of material whenever possible.

Now that you’ve ID tested those three lots, the next time you get a shipment of Vitamin C, it has two lots; A470 and C220. Provided you have it written in your inspection SOP correctly, you would not need to ID test lot A470 again since you’ve already tested it, but you would need to test C220. Make sense?

The next thing to look at is how to do the ID testing. Since no one test or examination will give you all the identity information you need, you really have to know your materials well to specify what test or examination you will do. I once talked with a client who was struggling with how to test one of his incoming materials. He used broccoli in one of his powders. Yup, raw broccoli! He bought fresh broccoli, dehydrated it, then ground it into a powder and used that in his product. We made the examination simple – if you have raw broccoli, a visual and organoleptic test will definitely identify the material as broccoli since nothing else will look and taste like raw broccoli. If he were to buy the broccoli all dried and powdered, then his test would be different. Then he would need a more complex method like FTIR, HPLC, or some other way to detect the chemical markers that provide broccoli’s unique fingerprint. You must spend the time to get to know your materials well so that you can pick the test or examination that will provide you with certainty that the material is in fact what it needs to be. That may be an HPTLC test or it could be a simple microscopic analysis. The thing is, you get to decide what the test is, as long as you can show it is scientifically valid and will provide you with verification that the material is what it says it is. The regulations state that you can use, “gross organoleptic analysis, Macroscopic analysis, microscopic analysis, chemical analysis, or other scientifically valid methods” so as you can see, you have the ability to be creative with your identity testing. Just be sure whatever method you decide to use provides you with verification that the material is what it needs to be.

I’ll give you another example, back in my manufacturing days, the company I worked for used Zinc Oxide as an active ingredient for an OTC drug product. All OTC ingredients need to be identity tested also. The USP listed several different ways to identify this material. One of them was that when heated strongly, zinc oxide would turn from its original white powder form to a yellow powder, then return to white when cooled. I could have sent the material out for IR testing or another form of chemical analysis, but instead, we specified that heat test as the ID test and it worked. It was scientifically valid, fast, and provided verification that the material was in fact what it needed to be. So you see, you can use a test that may seem too simple, but gives you the information you need. But you MUST spend the time getting to know your materials well first!

I hope this helps answer some of the questions out there.

Carol Brennon, ASQ CQA

What is Over-Granulating?

What is Over-Granulating?

What Exactly is “Over-Granulating?”

Over-Granulating results from using too much mechanical energy to mix the wet mass. It may also occur from mixing too long, past the end point. It may also occur from adding too much binding solution. Granules are created through a combination of mechanical energy and the quantity and addition rate of a binder. To some extent, it is also a result of the concentration of the binder in the solution. Over granulating is over processing or over working the powders while the liquid is being added and results in having a negative impact on the final tablet. An over worked granulation my not flow well, compress or eject properly. It may impact hardness, disintegration and dissolution profiles.

Determining Factors for Particle Size of Tablet Formulation

Determining Factors for Particle Size of Tablet Formulation

What are the determining factors for achieving the correct particle size distribution of a tablet formulation? I recall some 30 years ago being taught that the general rule of thumb is: particle size distribution needs to be small enough to go through an 18 mesh screen yet big enough as to not go through a 200 mesh screen. While machine type and condition play a role, the following list of items should also be considered.

Flowability: Generally speaking the smaller the particle the worse the flow. Compare powdered sugar with granular sugar. The fine small particles in powdered sugar aide dissolution but not flow.

Feeder clearance: Particle size must be larger than the feeder clearance to prevent leakage.

Die table run-out: If die table run-out increases, feeder clearance and particle size must also increase proportionately. To check run-out, use a dial indicator to determine the variation of the die table.

Die fill: Wide variations in particle sizes can cause inconsistent fill volumes.

Weight control: Final volume is final weight. Larger particles pulled out of the die can reduce the final weight. Fine particles require more precise scrape-off and increase the need for a good scraper blade.

Compressibility: Improves with increased particle size and decreases as particles become smaller and smaller. Small particles have less ability to lock together during compaction.

Hardness: Smaller particles are more sensitive to over-compression.

Ejection force: Small particles decrease interstitial space and increase drag and friction.

Lubrication levels: In general higher percentages of small particles require increased quantities of lubricant. Magnesium stearate is the most commonly used lubricant and should be de-agglomerated before use.

Disintegration & Dissolution: Small particles decrease disintegration time, and increase dissolution.

Friability: Larger particles usually lock together better which results in reduced friability while small particles often increase the potential for failure (higher friability).

Electro Static effects: Electro static charge is increased as the percentage of small particles increases.

Dust control: Fine particles create a dusty operation, creating a need for frequent production stoppages and press clean-ups.

Environmental conditions: Many products are hygroscopic and sensitive to heat. Variations in room conditions can result in poor flow, compression and ejection conditions.

Lamination & Capping: Small particles are the heart of the most common defects.

Punch lubrication: Dust and super fine particles become airborne and combine with the oils and greases which can produce black specks in tablets.

Tooling condition: Punch tip & die clearance are designed to control air release allowing for improved compaction.

Machine condition: Cleaning and maintenance are downtime issues. A high percentage of fine particles and dust increases the potential for greater wear, increased cleaning frequency, reduced yield, greater particle segregation, and more tablet defects.

Cost: Fines (small dusty particles) increase operating costs, require increased levels of dust collection, decreased yields, increased frequency of cleaning, and generate greater machine & tool wear. Reducing fines will improve tablet quality.

Summary: Establishing an appropriate particle size distribution will improve tablet quality and will reduce overall costs in the long run. Fine dusty particles are the source of most tablet defects.



Certified? We have had several customers ask recently about the new Dietary Supplement GMP’s, and one of the most misleading rumors has been that companies need to be certified or have some kind of “FDA certification”. This is simply not true. The FDA does not, and will not come to your facility and certify that you are compliant. They will inspect your facility and evaluate your level of compliance to the official GMP regulations.

To add to the confusion, there are several companies that do provide “certification”, like NSF. The FDA has not provided approval for NSF to go to companies and certify them…they simply do not do that. Just because you are certified by a company like NSF does not mean you will be compliant with current FDA GMP’s. It only means you are certifying that you have met the NSF requirements, which has turned into a marketing tool. Just look at the ads and company’s propaganda and see how many say they are NSF GMP Certified. I’m not saying that NSF, or other companies that provide “certification” are not providing a good service, they are! I’m simply trying to make it clear that being certified by anyone does not mean a company will meet the FDA’s GMP regulatory requirements and suddenly become compliant.

Our goal has been, and continues to be, helping manufacturers understand what it means to become FDA compliant and remove the confusion. Our “GAP” analysis is the best place to start and this is something we can help you with. A GAP analysis simply establishes where a company is now, and where they need to be. We help to develop on-going strategies to meet or exceed cGMP’s. The little “c” in “cGMP’s” stands for “current”, meaning that companies cannot just complete a few tasks and thus, they have arrived and can be certified; no such thing. A company must develop an on-going philosophy of continuous quality improvement.

So what do you need to do? In 2 ½ hours you can get a much better grip on it by listening to our session on Dietary Supplement GMPs 101 – New Ruling at Then call us and find out what a GAP Analysis audit can do for your company.

Is your tablet capping?

Is your tablet capping?

Last week we had some really good participation for our Tablet Capping webinar…thanks to all that attended.  This is one of those defects that can be really frustrating because once you feel you have a product figured out, and have it fine tuned, suddenly capping occurs. Getting the air out from between particles without moving the “fines” to the “air evacuation point is the key to success”.  During compaction as the upper punch tip enters the die, air is being pushed out of the die.  The design of the upper punch tip being smaller than the lower creates an avenue for air to escape. I call the point between the upper punch cup edge and the die wall the point of “air evacuation”.  As the air moves and evacuates it takes with it many of the dusty, fine, dry, light, non-compressible particles.  These particles can form a line along the point of air evacuation between the top of the tablet (aka the “Cap”) and the “Band” of the tablet, forming a line of non-compressible particles, which results in the “cap” not adhering to the rest of the tablet. The use of pre-compression is to lightly tamp or lock the small particles in place so they cannot migrate during final compression.  Upper punch penetration is another tool most modern machines have; adjust it as high as possible and the air will have a shorter distance to travel allowing for more complete air evacuation.  Machine speed can also play a roll to prevent capping because the time to evacuate the air is related to the clearance between the upper punch tip and the die wall and the depth of punch penetration…basically slowing the press gives the air more time to leave without pushing the fines to the air evacuation line which will result in capping.  If you want to fix capping…

  1. Optimize weight control
  2. Reduce Punch Penetration (2-3mm)
  3. Use pre-compression to lightly tamp
  4. Slow the press down until capping stops
  5. Add a taper into the die
  6. Change the radius of the upper punch tip to a compound radii
  7. Use a machine with 2 pre-compression stations (like a Manesty Nova)
  8. Reduce the percentage of fines within the formula.

Never change more than one item at a time and test to see the result.  Call or write to me if you need me to clarify any of this information.

Humidity & Temperature in Tableting

Humidity & Temperature in Tableting

RH…relative humidity & temperature in tablet manufacturing must be “constant”…variations are what cause so many problems.  There is no one perfect number for all products as the nature of raw materials is so different. Each and every powder reacts differently to temperature and humidity.  For some products very dry air will cause segregation of ingredients, and too high of humidity for others will cause huge sticking problems.  The key is maintaining a constant temperature and humidity. Most companies have low temperature and average humidity in the early morning hours; but, as the day progresses, machines and rooms’ heat up, and humidity from the outside changes, this creates problems so much so that the way a product runs in the morning is completely different than how it runs in the afternoon hours.  I have customers that cannot run certain products on rainy days or when the temperature is too high…conversely I have customers who cannot run products when it is to dry.  The bottom line is that humidity & temperature must remain as constant as possible…so look at when your product is most successful and when it is troublesome and you will have established parameters to guide you and to use as a caution to avoid problems.



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