Progress 10/01/10 to 09/30/11
Outputs
Progress Report Objectives (from AD-416) ARS is interested in developing a validated method for vitamin B6. The Cooperator is interested in developing validated methods for the determination of vitamins in dietary supplements and has contracted with AOAC INTERNATIONAL to select the best candidate methods. An Expert Review Panel (ERP) assembled by AOAC INTERNATIONAL, selected the method submitted by the Food Composition and Methods Development Lab (FCMDL) for development as the best candidate vitamin B6 method. Approach (from AD-416) FCMDL will modify the candidate method based on the recommendations of the ERP with respect to sample extraction. FCMDL will then characterize the precision, stability, robustness, and accuracy of the modified method as required by AOAC INTERNATIONAL for SLV methods. FCMDL will further characterize the method for it�s suitability for accurate analysis of other water-soluble vitamins. FCMDL will submit the method to AOAC INTERNATIONAL for a full collaborative study and adoption as an official method. During the period of this agreement, a method was developed for the determination of vitamin B6 in vitamin and mineral supplements. A general extraction method was used that was modified slightly depending on whether the supplement was a tablet, soft gel, liquid, sustained release material, or a �gummy-bear� material. Chromatographic separation was based on both high performance liquid chromatography (HPLC) and ultra- HPLC (U-HPLC). The U-HPLC separation was accomplished in less than 20 minutes. The vitamin was detected using ultraviolet absorption, fluorescence, and mass spectrometry. Accuracy and precision of �5% were achieved for all supplement materials. This agreement was monitored through routine conversations and email communications with NIH/Office of Dietary Supplements.
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Progress 10/01/09 to 09/30/11
Outputs
Progress Report Objectives (from AD-416): ARS is interested in developing a validated method for vitamin B6. The Cooperator is interested in developing validated methods for the determination of vitamins in dietary supplements and has contracted with Association Official Analytical Chemists (AOAC)INTERNATIONAL to select the best candidate methods. An Expert Review Panel (ERP) assembled by AOAC INTERNATIONAL, selected the method submitted by the Food Composition and Methods Development Lab (FCMDL) for development as the best candidate vitamin B6 method. Approach (from AD-416): FCMDL will modify the candidate method based on the recommendations of the ERP with respect to sample extraction. FCMDL will then characterize the precision, stability, robustness, and accuracy of the modified method as required by Association Official Analytical Chemists (AOAC) INTERNATIONAL for Single-Laboratory Validation methods. FCMDL will further characterize the method for it�s suitability for accurate analysis of other water-soluble vitamins. FCMDL will submit the method to AOAC INTERNATIONAL for a full collaborative study and adoption as an official method. This project was only kept open for closeout purposes. There is no research to report.
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Progress 10/01/09 to 09/30/10
Outputs
Progress Report Objectives (from AD-416) ARS is interested in developing a validated method for vitamin B6. The Cooperator is interested in developing validated methods for the determination of vitamins in dietary supplements and has contracted with AOAC INTERNATIONAL to select the best candidate methods. An Expert Review Panel (ERP) assembled by AOAC INTERNATIONAL, selected the method submitted by the Food Composition and Methods Development Lab (FCMDL) for development as the best candidate vitamin B6 method. Approach (from AD-416) FCMDL will modify the candidate method based on the recommendations of the ERP with respect to sample extraction. FCMDL will then characterize the precision, stability, robustness, and accuracy of the modified method as required by AOAC INTERNATIONAL for SLV methods. FCMDL will further characterize the method for it�s suitability for accurate analysis of other water-soluble vitamins. FCMDL will submit the method to AOAC INTERNATIONAL for a full collaborative study and adoption as an official method. The FCMDL vitamin B6 method developed at FCMDL, based on liquid chromatography, ultraviolet, florescent, and mass spectrometric detection, was chosen as one of twelve methods by an AOAC expert Review Panel (ERP) to be included for development as one of the �World Class� methods being developed by AOAC under an NIH/FDA/AOAC contract for methods for vitamin analysis in dietary supplements. This interagency agreement is to jointly carry out optimization and further develop a formal Single Laboratory Validation Study, extending the Vitamin B6 method to a wider variety of dietary supplement formulations. A progress report on this activity was given at the 124th AOAC annual meeting, September 2010. This agreement was monitored through routine conversations and e-mails with AOAC International and the Office of Dietary Supplements.
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