Testing is more than a necessary evil; it is part of the regulatory requirement for compliant manufacture of dietary supplements. Failure to test or testing using inappropriate, unqualified methods can render a dietary supplement adulterated just as much as if the wrong ingredient were used, which also carries the same regulatory consequences. The regulations describe multiple requirements for testing, with the three primary requirements being:
- Finished product brands must test against specifications that they establish.
- Results must be obtained using scientifically valid, analytical methods.
- Brands must test every batch of components, in-process materials and finished goods.
Brands must create standards that apply to testing the components and products, along with specifications for each parameter of interest. These must include evaluations to ensure identity, purity, strength and composition of the component, in-process material and finished product. This must also include specifications for known contaminants that might be present in products. Once done, these specifications serve as the basis for required testing.
Methods used should be identified in the specification. The regulatory requirement is they must be “scientifically valid analytical methods.” The meaning of this phrase is not specifically defined in the regulations and, during rulemaking, discussion of the term involves only notation of potential sources for such methods. Regardless of where the test is performed, whether in-house or by a contracted laboratory, it is a regulatory requirement to ensure methods meet this undefined standard. If testing is performed in-house, methods must be developed in nearly all instances. This development requires documentation of the steps taken to demonstrate the scientific validity of the method before employing it in the control and release of product. Application of a compendial method (USP, for example) or a validated method ( AOAC methods) is rarely directly and completely appropriate for the material being tested. As components are processed into a finished dietary supplement, the unmodified application of official or compendial methods decreases. Changing sample preparation alone results in a variance from the methods, and requires documented work to demonstrate the appropriateness of even small changes. Assurance is achieved through documented work to verify the method is suitable and applicable to the sample type, including when instrumentation is used and qualified on the specific instrument. Each of these aspects need to be documented by the lab doing the testing. This requires work, and when using a contract lab, brands need to verify that such work has been done before accepting the results.
Qualifying the laboratory to do the work is another necessary step in compliance to ensure results are gathered using methods that meet the standard for scientific validity. No documentation of method validity presents a shortfall in compliance, when considering the applicable, if undefined, standard. While no regulatory enforcement has occurred on third-party labs and the methods used, the obligations regarding documented validity of methods used remains. The scientifically valid standard does not mean every method is validated within scientific circles. It does mean, however, determining the applicability of any method used in the control and release of dietary supplements must be affirmed either by the nature of the method (strict adherence to compendial or official methods) or through a process of affirming method validity. In either instance, documentation of such determinations must also be present.
The third primary consideration—the general rule—is every batch (or lot) of components, in-process materials and finished product must be tested against specifications. The exceptions to this are within a narrow range (components supplied by a vendor deemed to be “qualified to supply” a component, some finished goods testing and tests for which there is no scientifically valid method). Since each batch or lot must be tested to some degree, the balance is in determining what tests to perform against costs associated with the needs to meet the regulatory standard.
Lab standards are broadly identified. Laboratory operations involve a series of requirements for everything from housekeeping and environmental monitoring to documentation of the scientific validity of the methods used. These standards, even in the absence of a specific definition, apply regardless of whether testing occurs within the company or at a contracted laboratory. Ensuring compliance means verifying the necessary work is done to demonstrate conformance to the standards and, thereby, compliance.
As chief operating officer, Jim Lassiter oversees all consulting operations at Ingredient Identity. He has more than four decades of experience in quality control (QC), and government and regulatory affairs throughout the pharmaceutical, dietary supplement and natural product industries with organizations such as Nutrilite, Robinson Pharma, Irwin Naturals, Chromadex, the American Herbal Products Association (AHPA) and the Council for Responsible Nutrition (CRN). A respected author and speaker, Lassiter has served on numerous industry and trade boards.