Quality Focus: The Laboratory Notebook

Answering important questions about quality.

By Robert Green

In January of 1999, I wrote an article with the following lead: “Quality. If there is one word that describes the most important issue facing the nutritional supplement industry today it is ‘quality.’” Now, two years later as I use it to open the first column in Nutraceuticals World on quality, it still rings true.

Our industry is built on consumer confidence in our products. If we shake that confidence our industry collapses. The popularity of our products have made the instances of questionable quality more newsworthy and many have seized this opportunity to jump into the limelight. Indeed, some have created businesses around it. So bad news travels fast. But even more fundamentally, we all have an obligation to the consumer to produce and sell only quality products. After all, our products are intended for human ingestion.

So what do we do? The answer is obvious; take the appropriate steps to insure the quality of our products. Not an unreasonable position. Ironically, as soon as this occurs the self-appointed testers will go away.

At Integrated Biomolecule we see thousands of samples, both raw materials and finished products. On any given day we see the good, the bad and the ugly. While there are certainly instances where the bad and the ugly are attributable to scoundrels, in most instances these problems result from well-intentioned parties with insufficient knowledge and limited access to technical expertise.

That’s where this column fits in. Now you have a place to send your questions and we will answer some in each column. It’s free advice, and hopefully the old adage of “you get what you pay for” won’t apply here.

As for the column’s title, a “laboratory notebook” is an essential tool of all lab personnel as it is a written record of important laboratory events. Hopefully, this column will serve as a written record of important quality issues facing our industry today. So on to the first question.

Is it still a problem that there are no industry-recognized analytical methods and therefore different labs may use different means to test the same sample?

Yes and no (remember, this advice is free). Life would be easier for all of us if a recognized testing method was established for each product. With the multitude of products and the various forms they take, this will not happen. (Keep in mind, a method to test an individual raw material may not work when that ingredient is in a single-component capsule with excipients/flow agents or a multi-component capsule with other active ingredients, so the job is staggering.) Nevertheless, while this situation may have been a serious problem in the industry’s early years, in our daily world we no longer see it as such.

Through the years analytical labs on the whole have gotten much better. Analytical methods have been refined, and, at least at the more conscientious labs, validated in-house. As a result, the quality of the best labs is now first rate. We find that the quality labs are generally using the same methods with some minor modifications that have no effect on the end result. Why? Because we are all striving to do the best job possible, and since analytical chemistry is a science, we all generally get to the same point.

Moreover, when there is a difference of opinion between quality labs, technical information is exchanged and we learn from each other. Since analytical chemistry is a science, two professionals can objectively look at two different methods and select the more exacting one, which is then used to settle the dispute. In the end, the analytical data will speak. Either the sample is good or bad; there is a correct answer.

Interestingly, since such a big deal on the potential problems of differing methods was made in the past some have seized upon this as the knee-jerk reaction to an unfavorable lab result. Too many times the head of sales and marketing of a supplier on the wrong side of an analytical report will call to assert (quite vociferously) that the lab doesn’t know what it’s doing and that it used the wrong method. When asked what method he/she thinks was used you get the traditional response, “Well I’m not the technical person.” Funny thing is, when asked to provide the analytical data that contradicts the lab’s results generally nothing arrives, which we surmise means the material was not previously tested.

So the moral of the story is make sure you use a conscientious analytical lab that validates its methods, discloses the analytical methods used (more on this later) and acts in a professional manner to resolve any disputes. Otherwise, you will get analytical results but they may not serve your purpose.

My analytical lab refuses to disclose the methods by which my analyses are conducted. They claim the methods are proprietary and confidential. Is this true?

Anyone can claim anything they like, but this position, which is surprisingly common in the supplement industry, is wrong. The underlying principal in analytical chemistry is that on any given day any competent lab can duplicate the results of another lab. This can only be accomplished when labs disclose the methods of analysis. Any lab that refuses to disclose methods violates this basic tenet, and in our mind, should not be charging money for analytical services.

Apropos of the preceding question, in the case of an analytical dispute, a lab refusing to disclose its method of analysis precludes the essential technical discussion. The discussion quickly deteriorates into a non-technical argument. In analytical chemistry the data speaks…if you don’t share the data you can’t speak. If your lab won’t disclose the technical information then you lose the dispute.

Keep in mind there is a difference between the analytical method used and the actual protocol followed. The analytical method is the general description of the analysis, such as the equipment used, its settings, etc. This is all an analytical lab needs to duplicate the analysis.

The protocol, on the other hand, is the step-by-step procedure (sometimes fondly referred to as the “recipe”) followed by the lab to conduct the analysis. It is not required to duplicate the analysis and it may indeed contain proprietary techniques that a lab will not share.

A lab that keeps its method secret violates the very essence of analytical chemistry and will not support you in the event of a controversy concerning a sample. Besides, if they won’t tell you how their work was conducted, how do you know they actually did it? You should steer clear of labs that won’t disclose the method used to test your products.

I have a certificate of analysis from my supplier showing the material I am buying meets specifications. Can I rely on this?

Maybe (don’t forget this is still free advice). A certificate of analysis (C of A) is nothing more than a piece of paper with some writing on it. Anyone can prepare a C of A. The key question is what’s behind that writing.

The C of A is supposed to report the results of the various tests listed on it. There must be actual analytical data supporting each item. So, for example, the fact that a C of A states your chondroitin sulfate is 93% pure is nice, but there also must be in existence an HPLC chromatogram or other analytical data which proves the material in question is indeed 93% pure. You have a right to see that data.

If you are receiving a C of A from a major pharmaceutical company and you are convinced the material it describes is the material in your hands, then that C of A may be given great weight. If, on the other hand, the C of A comes from a foreign manufacturer you never heard of or a middleman you know has no analytical capabilities or expertise, you need to take great care.

And never forget, much can happen between the time the material leaves the manufacturer and arrives on your doorstep. That’s why you must always be wary, and testing is very cheap insurance.

That’s it for our first edition of The Laboratory Notebook. Please send your questions to my email address. Until then, make quality your number one priority.

NW

Robert S. Green is the president of Integrated Biomolecule Corporation, a biotechnology company that conducts nutritional supplement ingredient and finished product testing and provides research, development, production and technical marketing services. He can be reached at 520-799-7566; Fax: 520-799-7562; E-mail: [email protected]; Website: www.integratedbiomolecule.com.