The Analytical Methods Program is the largest component of ODS's Dietary Supplements Analytical Methods
and Reference Materials (AMRM) Program. A large community of academics, regulators, manufacturers, laboratories, and trade associations
is interested in developing and validating analytical methods for dietary supplements.
Program Need: Very few publicly available and reliable analytical methods for dietary supplements exist. This makes it
difficult to confirm ingredient identity or product composition and to conduct adequate clinical studies assessing safety and efficacy.
Furthermore, the Dietary Supplement Health Education Act empowered
FDA to establish current
good manufacturing
practices for dietary supplements. The law requires that any enforcement action taken against dietary supplement products use publicly
available methods.
Goal: The goal of this AMRM program component is to develop and validate methods that identify and quantify ingredients
(bioactive and other chemical markers, adulterants, or contaminants) in dietary supplements.
Description: To achieve this goal, ODS collaborates with
FDA, NIST,
USDA, AOAC International, and other organizations.
Under the auspices of the AMRM program, ODS and FDA have supported
AOAC International
in developing an infrastructure
to support methods validation. AOAC International is a not-for-profit voluntary consensus standards body cited in the US Code of Federal
Regulations and recognized by international regulatory and scientific institutions.
AOAC International maintains a committee structure to find and validate methods for dietary supplement ingredients. Criteria for prioritizing
the need for methods are based on stability of market share, availability of reference materials and suitable methods, scientific and regulatory
need, and industry interest. Urgent public health needs, e.g., the safety of ephedra, drive prioritization. Following prioritization, available
methods are subjected to a peer-review process by committees composed of experts from industry, academia, and government. The committees select
the most promising methods for further development, optimization, and validation. ODS supports their
development and validation through a variety of funding mechanisms. AOAC International evaluates the validation study results and publishes the
methods in the Journal of AOAC International. It also gives official sanction to acceptable methods if they meet AOAC's standards; they
then become AOAC Official Methods of AnalysisSM (OMA).
ODS also supports FDA and USDA in methods development and optimization. FDA has been developing methods for detecting and quantifying
contaminants (e.g., mycotoxins, toxic elements, and pesticides) found in source material and finished products. USDA is working on methods
for quantifying phenolic glycosides and is evaluating methods for determining the authenticity of botanicals by principal component analysis.
NIST may also develop and validate methods in its process of certifying values in
NIST Standard Reference Materials® (SRM) and calibration standards. ODS provides support for
the development of SRMs.
Validated Methods Defined: A validated method is a method that has been systematically evaluated for reliability and accuracy.
Methods can be validated in single laboratory or multiple laboratories.
Types of Validation: A method that is intended to be performed in only one laboratory can be validated within that laboratory.
This would be a single-laboratory validation (SLV). However, the results of a SLV method can not necessarily be compared to results obtained
using a different method or the same SLV method in a different laboratory. The SLV method can be considered the first step toward a full
official method validation. The SLV method debugs the method before it is subjected to a
collaborative study.
The collaborative study is the gold standard. Multiple laboratories perform the same test on the same samples. If results from most of
the laboratories are the same, the collaborative study is successful. A successful collaborative study leads to listing the method as an
OMA.
To date, the ODS AMRM Program has supported SLV studies that lead to collaborative studies. Early in the AMRM program emphasis was placed
on creation of OMA. In the future, ODS will place more emphasis on SLV studies. ODS stakeholders will determine whether an OMA is needed.
Availability of Validated Methods: The ODS Web site lists the ingredients for which validated methods are published.
Their citations are referenced and ingredients for which validation testing is ongoing are also listed. Only ingredients with ODS-supported
methods validation are listed. ODS AMRM Program stimulated the field of methods validation for dietary supplements, and many more validated
methods now exist. These methods can be identified by searching the AOAC International Web site for methods published in the
Journal of AOAC International or OMA.
How to Become Involved: The AOAC International provides training materials for and courses on designing and conducting
validation studies. It also requests nominations of dietary supplement ingredients for consideration of methods validation. AOAC International's
website has further information about these opportunities.
When funding opportunity announcements for methods development are available, ODS posts them on the
AMRM Program Website.