Analytical Methods and Reference Materials
Description Current Research Initiatives Program Accomplishments Projected Future Initiatives
The rapid expansion of the dietary supplement marketplace has resulted in a proliferation of ingredients and products and outstripped the pace of development of reliable analytical methods. Precise, accurate and rugged analytical methods and reference materials are essential for verification of ingredient identity, identifying and measuring contaminants, and measuring the amounts of declared ingredients in raw materials and finished products. The Dietary Supplements Methods and Reference Materials Program was created in 2002 in response to direction from the U.S. Congress. It is a broad-based initiative that supports the technical aspects of methods development as well as the administrative and consensus building foundation necessary for advancing the field. The Program supports critical laboratory research and the infrastructure necessary for evaluation and dissemination of new methods and reference materials. Continued expansion of this program is anticipated as emerging science identifies new needs and opportunities. Responding to the Congressional mandate, ODS held two stakeholder meetings in 2002. Attendees expressed strong support for the program and made several specific recommendations (Saldanha et al., 2004, J AOAC Int. 87:162-5
). An additional stakeholder meeting was held in September 2007. A summary of this recent stakeholder meeting will be available later in 2008. An overview of the ODS Analytical Methods and Reference Materials Program for Dietary Supplements was published in the May 2007 issue of Analytical and Bioanalytical Chemistry
(Betz JM, et al., 2007, Anal Bioanal Chem 389:19-25
Current Research Initiatives
- The ODS is co-funding with the FDA's Center for Food Safety and Applied Nutrition (CFSAN), a contract with AOAC International to create 15 AOAC Official Methods of Analysis for Dietary Supplements.
- ODS is funding an Inter-Agency Agreement (IAG) with the National Institute of Standards and Technology (NIST) that calls for production of suites of matrix reference materials (keyword search: "dietary supplement") and the development and implementation of a pilot "Quality Assurance Program for Analysis of Dietary Supplements."
- ODS is funding an IAG with USDA's Food Composition Laboratory for the purpose of developing and optimizing analytical methodology for the extraction and determination of antioxidant flavonoid glycosides and for developing methods for chemical fingerprinting and chemometric techniques as bases for establishing botanical identity.
- ODS is funding an IAG with FDA/CFSAN for the purposes of developing, optimizing, and validating analytical methods for toxic elements, pesticides, and certain mycotoxins that have been reported as contaminants in some dietary supplements.
- ODS is funding research and development as well as production and dissemination of calibration standards and analytical reference standards.
- A study for validation of thin layer chromatographic fingerprinting methods for determining botanical identity of 15 herbs in commerce, an electronic herbarium pilot project, production of a handbook of botanical microscopy are in process.
- Nine supplement methods have been collaboratively studied, with seven approved as first action Official Methods of Analysis.
- Seven additional collaborative studies are in progress.
- Nine single laboratory validation studies have been performed and published. An additional seven single laboratory validation studies are in progress, with 38 additional ingredients in various stages of study.
- The past five years have seen the emergence of a community of analytical chemists, dietary supplement researchers, and others concerned with dietary supplement analytical methodology. In the two years before the launch of the ODS program, there were no dietary supplement publications in the Journal of AOAC International. Between the launch of the program in 2002 and January 2007, there have been approximately 100 dietary supplement methods published in the journal, about 20 per year.
- ODS has funded production of very high purity standards for use as calibration standards. To date, the program has contracted for the production of nine USP reference materials and approximately 20 other materials have also been produced for use in collaborative and pre-collaborative studies.
- Five suites of NIST Standard Reference Materials (SRMTM) have been produced and certified.
Projected Future Initiatives
- The current research initiatives will be continued and as progress is made, additional tasks will be added as appropriate.
- There will be increased emphasis on single laboratory validation studies and on performance-based analytical methods development. The NIST IAG will continue and expand the pilot "Quality Assurance Program for Analysis of Dietary Supplements."