How to Handle Unfavorable Analytical Results
by Robert Greens
As a responsible member of the nutritional supplement industry, you sent a sample of a product you are handling (be it a raw material or finished product), to an analytical laboratory for testing and the results are not what you had expected. Now what?
Don't panic. Negative analytical results are expected; that's why products are tested in the first place. If everything was perfect there would be no need for testing. That's why Good Manufacturing Practices (GMPs) anticipate problems by requiring that quality testing and procedures are in place to handle them, once discovered.
Negative analytical results are just the start of a quality assurance process; at this point you have no way of knowing how it will end. Maybe the material is in fact acceptable. Perhaps the material was indeed deficient, in which case you may have saved your business significant economic and reputation losses. While no one likes bad news, it is better to discover it early and take corrective action rather than blindly walk into a much bigger problem.
Determine how negative the negative results really are. There is always room for leeway. If your St. John's wort extract should be 0.03 percent Hypericin and the analytical result says 0.0297 percent, it's safe to assume the material is acceptable. Just how far off the results can be is dependent upon the product and other factors, but a 1 percent or 2 percent variance is generally acceptable.
In addition, certain analytical methods are more selective than others. For example, a lower result from an HPLC analysis (which is very selective) may not contradict a higher result from an ultraviolet (UV) analysis (which is less selective).
Let's say your product's deficiency exceeds an acceptable range. The next step is to confirm that the analysis is correct, and this has two prongs: the sample and the analytical laboratory. Review where the sample came from and how it was collected. As described in our "Correct Sampling" article [June 28, 1999 issue of the Natural Products Industry Insider], the entire analytical testing process is dependent upon the use of a correct sample. The sample must be from the same material now at issue, and it must have been collected in a manner which insures it is representative of the entire product batch. If you scooped the sample from the top of a 50-liter drum so that it is not representative of the entire contents of the drum you may now regret that, for it may be the cause of the problem.
You also must convince yourself that the analysis is correct. Call the laboratory and quiz them on their work. Non-technical folks get intimidated when talking to labs, but you pay good money for an analysis and the lab has an obligation to discuss it with you on terms you understand.
Ask the lab how often they test the product in question; if the answer is "not often" you have cause for concern. Find out what method they used (e.g. HPLC, GC, LC). Find out where the procedure they followed came from (e.g. published paper, in-house).
Ask if the lab validated the method they used (i.e. ran it many times under controlled conditions to insure it works consistently) and where they obtained the standard (another sample of the product which is deemed perfect and against which your product is judged). Ask for a copy of the readout made by the instrument that conducted the analysis (as opposed to the product analysis report, which generally only recites the results) and have it explained to you. As a paying customer, you have a right to this information. All of these questions are general and the answers can easily be explained to the lay person. If at the end of the conversation, you still don't understand the situation, something is wrong.
If you are convinced that both the sample and analysis are correct, then most likely it's the old adage: if it looks like a duck and quacks like a duck it must be a duck. But you are not finished. Let the party responsible for the deficiency know that you will not stand for inferior material. Whether it is an ingredient supplier who sold low-grade material or an encapsulator who missed the correct formulation, the sale of deficient material is never acceptable. It certainly cannot be the case in our industry where the products are destined for human consumption.
No doubt one day you will find yourself in a situation where you and the other party in your transaction have conflicting analytical results. After you go through the above exercise with your lab, you then need your lab to go through the exercise with the other party's lab. While many labs cooperate in these situations, others may not; they may get defensive and argumentative. It is in your interest to resolve the dispute; do not fight. In this situation you should instruct your lab to act in your best interest and be cooperative, with the goal of resolving the problem.
Negative analytical results should neither be feared nor ignored. They are a fact of life and should be acted upon in a professional and methodical fashion by both the party who requested the analysis and the laboratory that conducted it. This is good business for the concerned parties, the industry as a whole and consumers on whom we are all dependent.
Robert S. Green is the President of Integrated Biomolecule Corporation, which conducts analytical testing and research and development of nutritional supplements. He can be reached at (520) 799-7566 or by fax at (520) 799-7562.