Steven Dentali, PhD, Botanical Industry Consultant03.01.17
In my comments on the State of the Industry Update & Outlook for 2017 (Nutraceuticals World, December 2016), I was hoping to educate companies that may not know about certain resources and standards, while also encouraging continued and increased engagement from those already leading the way to authenticate products up and down the supply chain. I mentioned the “specifications-results-certificates of analysis triad” and I’d like to explain more about what that means.
The Triad
Manufacturers are familiar with ingredient specification sheets and certificates of analysis (CoAs), as regulations require attention to these documents. Sometimes that attention can simply be paper pushing, which is alright as long as there is adequate assurance that those specifications are meaningful. Specifications must be testable by scientifically valid methods, and actual test results must be reported on certificates of analysis. Specs are more than just ingredient descriptions.
Specifications detail how a product (or ingredient) must perform when tested by valid tests. A certificate of analysis presents actual test results, tying specifications to the CoA and thereby verifying that the specifications are met. Specification sheets may also contain information that is not subject to a test and for which no analytical test can be performed. Information for which no test result is reported (e.g., botanical extract ratios) don’t technically belong on a specification sheet, however, this is a minor issue relative to assuring that specifications are met via appropriate testing with results reported on CoAs.
Specifications should include the test method to be used to verify that the specs are actually met. CoAs are not meaningful without referencing the test method used or without access to the actual test’s raw data results. Oddly, it is not uncommon to see such tests identified as HPTLC, HPLC, NMR, NIR, or organoleptic with no reference to any actual test method. These are technologies, not test methods. They don’t provide enough information on what test was used any more than “oven” is sufficient information on how to bake a cake. They don’t identify a valid test method just as “heat” or “knife” doesn’t tell anyone how to make dinner.
Test results themselves are only as good as 1) the scientific validity of the test, 2) proper functioning of the equipment and its calibration, and 3) the proficiency of the laboratory/person running the test. External standards, instrument performance and personnel training matter here because scientifically valid results require that the test method, the equipment to run it, and the person running the method all must themselves be tested. It is incumbent upon manufacturers to understand and manage these requirements or work with people who do.
Engaging with Partners
This brings us back to industry associates and supporters who are now our active participants and willing partners for testing integrity. AOAC INTERNATIONAL is actively engaged with industry as it publishes Official Methods of Analysis applicable to supplement ingredients. Its Stakeholder Panel on Dietary Supplements process, supported by the Office of Dietary Supplements (ODS) at the National Institutes of Health, is open to volunteers who suggest materials for which validated methods of analysis are needed. Volunteers also determine what those methods should be able to do, and which ones actually meet those performance requirements. A specification becomes meaningful when it moves from “HPLC” to an actual official method with worldwide recognition.
Laboratory performance isn’t necessarily tied to using specific methods. If a lab can produce acceptable results (meaning accurate results, not necessarily the desired ones) by a method of their choosing, that’s ok too. The Dietary Supplement Laboratory Quality Assurance Program run by the National Institute of Standards and Technology in collaboration with ODS allows companies to test the integrity of their results using supplied materials with defined targets. They also provide standard materials.
If your company, suppliers, testing laboratories and customers already know about and are engaged with these efforts, as appropriate, then great. If not, my suggestion would be to take time to chat with representatives at the Natural Products Expo West in Anaheim, CA, in March. While you’re at it, don’t forget to have conversations with the American Botanical Council (ABC), the U.S. Pharmacopeial Convention (USP) and other educational foundations and standards-setting organizations, including the industry trade associations. Together we can build a stronger industry.
The Triad
Manufacturers are familiar with ingredient specification sheets and certificates of analysis (CoAs), as regulations require attention to these documents. Sometimes that attention can simply be paper pushing, which is alright as long as there is adequate assurance that those specifications are meaningful. Specifications must be testable by scientifically valid methods, and actual test results must be reported on certificates of analysis. Specs are more than just ingredient descriptions.
Specifications detail how a product (or ingredient) must perform when tested by valid tests. A certificate of analysis presents actual test results, tying specifications to the CoA and thereby verifying that the specifications are met. Specification sheets may also contain information that is not subject to a test and for which no analytical test can be performed. Information for which no test result is reported (e.g., botanical extract ratios) don’t technically belong on a specification sheet, however, this is a minor issue relative to assuring that specifications are met via appropriate testing with results reported on CoAs.
Specifications should include the test method to be used to verify that the specs are actually met. CoAs are not meaningful without referencing the test method used or without access to the actual test’s raw data results. Oddly, it is not uncommon to see such tests identified as HPTLC, HPLC, NMR, NIR, or organoleptic with no reference to any actual test method. These are technologies, not test methods. They don’t provide enough information on what test was used any more than “oven” is sufficient information on how to bake a cake. They don’t identify a valid test method just as “heat” or “knife” doesn’t tell anyone how to make dinner.
Test results themselves are only as good as 1) the scientific validity of the test, 2) proper functioning of the equipment and its calibration, and 3) the proficiency of the laboratory/person running the test. External standards, instrument performance and personnel training matter here because scientifically valid results require that the test method, the equipment to run it, and the person running the method all must themselves be tested. It is incumbent upon manufacturers to understand and manage these requirements or work with people who do.
Engaging with Partners
This brings us back to industry associates and supporters who are now our active participants and willing partners for testing integrity. AOAC INTERNATIONAL is actively engaged with industry as it publishes Official Methods of Analysis applicable to supplement ingredients. Its Stakeholder Panel on Dietary Supplements process, supported by the Office of Dietary Supplements (ODS) at the National Institutes of Health, is open to volunteers who suggest materials for which validated methods of analysis are needed. Volunteers also determine what those methods should be able to do, and which ones actually meet those performance requirements. A specification becomes meaningful when it moves from “HPLC” to an actual official method with worldwide recognition.
Laboratory performance isn’t necessarily tied to using specific methods. If a lab can produce acceptable results (meaning accurate results, not necessarily the desired ones) by a method of their choosing, that’s ok too. The Dietary Supplement Laboratory Quality Assurance Program run by the National Institute of Standards and Technology in collaboration with ODS allows companies to test the integrity of their results using supplied materials with defined targets. They also provide standard materials.
If your company, suppliers, testing laboratories and customers already know about and are engaged with these efforts, as appropriate, then great. If not, my suggestion would be to take time to chat with representatives at the Natural Products Expo West in Anaheim, CA, in March. While you’re at it, don’t forget to have conversations with the American Botanical Council (ABC), the U.S. Pharmacopeial Convention (USP) and other educational foundations and standards-setting organizations, including the industry trade associations. Together we can build a stronger industry.
