NISTIR 8203 Dietary Supplement Laboratory Quality Assurance Program: Exercise M Final Report Melissa M. Phillips Catherine A. Rimmer Laura J. Wood Maria R. Ale Charles A. Barber Hannah Stindt Lee Yu This publication is available free of charge from: https://doi.org/10.6028/NIST.IR.8203 NISTIR 8203 Dietary Supplement Laboratory Quality Assurance Program: Exercise M Final Report Melissa M. Phillips Catherine A. Rimmer Laura J. Wood Maria R. Ale Charles A. Barber Hannah Stindt Lee Yu Chemical Sciences Division Material Measurement Laboratory This publication is available free of charge from: https://doi.org/10.6028/NIST.IR.8203 February 2018 U.S. Department of Commerce Wilbur L. Ross, Jr., Secretary National Institute of Standards and Technology Walter Copan, NIST Director and Under Secretary of Commerce for Standards and Technology ABSTRACT The NIST Dietary Supplement Laboratory Quality Assurance Program (DSQAP) was established in collaboration with the National Institutes of Health (NIH) Office of Dietary Supplements (ODS) in 2007 to enable members of the dietary supplements community to improve the accuracy of measurements for demonstration of compliance with various regulations including the dietary This publication is available free of charge from: http from: charge of free available is publication This supplement current Good Manufacturing Practices (cGMPs). Exercise M of this program offered the opportunity for laboratories to assess their in-house measurements of nutritional elements (potassium and zinc), contaminants (arsenic and lead), water-soluble vitamins (thiamine (B1) and riboflavin (B2)), fat-soluble vitamins (total vitamin K1, cis- and trans-vitamin K1), botanical marker compounds (curcuminoids, chondroitin sulfate), and identity (chondroitin) in foods and/or botanical dietary supplement ingredients and finished products. KEYWORDS botanical; chondroitin; contaminants; curcuminoids; dietary supplements; foods; minerals; vitamins. s / /doi.org/10.6028/NIST.IR. 8203 i TABLE OF CONTENTS INTRODUCTION ...........................................................................................................................1 OVERVIEW OF DATA TREATMENT AND REPRESENTATION ...........................................2 Statistics ...............................................................................................................................2 This publication is available free of charge from: http from: charge of free available is publication This Individualized Data Table ....................................................................................................3 Summary Data Table ...........................................................................................................4 Graphs ..................................................................................................................................4 Data Summary View ................................................................................................4 Sample/Sample Comparison View ...........................................................................5 NUTRITIONAL ELEMENTS (POTASSIUM AND ZINC) IN SPINACH LEAVES AND SPIRULINA .....................................................................................................................................6 Study Overview ...................................................................................................................6 Sample Information .............................................................................................................6 Spinach .....................................................................................................................6 Spirulina ...................................................................................................................6 Study Results .......................................................................................................................7 Technical Recommendations ...............................................................................................7 Table 1. Individualized data summary table (NIST) for potassium and zinc in spinach and spirulina.........................................................................................................9 s Table 2. Data summary table for potassium in spinach leaves and spirulina. ..................10 / /doi.org/10.6028/NIST.IR. Table 3. Data summary table for zinc in spinach leaves and spirulina ............................11 Figure 1. Potassium in SRM 1570a Trace Elements in Spinach Leaves (data summary view –analytical method) ................................................................................12 Figure 2. Potassium in spirulina (data summary view –analytical method) ....................13 FIGURE 3. Zinc in SRM 1570a Trace Elements in Spinach Leaves (data summary view –analytical method) ................................................................................................14 Figure 4. Zinc in spirulina (data summary view –analytical method) .............................15 8203 Figure 5. Laboratory means for potassium in SRM 1570a Trace Elements in Spinach Leaves and spirulina (sample/sample comparison view) ..................................16 Figure 6. Laboratory means for zinc in SRM 1570a Trace Elements in Spinach Leaves and spirulina (sample/sample comparison view)................................................17 TOXIC ELEMENTS (Pb AND As) IN GINGER AND GINSENG DIETARY SUPPLEMENTS............................................................................................................................18 Study Overview .................................................................................................................18 Sample Information ...........................................................................................................18 Ginger Rhizome .....................................................................................................18 Asian Ginseng Rhizome .........................................................................................19 Study Results .....................................................................................................................19 Technical Recommendations .............................................................................................20 ii Table 4. Individualized data summary table (NIST) for lead and arsenic in ginger and ginseng dietary supplements ....................................................................................21 Table 5. Data summary table for lead in ginger and ginseng rhizome dietary supplements.....................................................................................................................22 Table 6. Data summary table for total arsenic in ginger and ginseng rhizome dietary supplements.....................................................................................................................23 This publication is available free of charge from: http from: charge of free available is publication This Table 7. Data summary table for total inorganic arsenic in ginger and ginseng rhizome dietary supplements ..........................................................................................24 Table 8. Data summary table for arsenic III in ginger and ginseng rhizome dietary supplements.....................................................................................................................25 Table 9. Data summary table for arsenic V in ginger and ginseng rhizome dietary supplements.....................................................................................................................26 Figure 7. Lead in SRM 3398 Ginger (Zingiber officinale) Rhizome (data summary view –analytical method) ................................................................................................27 Figure 8. Lead in SRM 3384 Ground Asian Ginseng (Panax ginseng C.A. Meyer) Rhizome (data summary view –analytical method) ........................................................28 Figure 9. Total arsenic in SRM 3398 Ginger (Zingiber officinale) Rhizome (data summary view –analytical method) ................................................................................29 Figure 10. Total arsenic in SRM 3384 Ground Asian Ginseng (Panax ginseng C.A. Meyer) Rhizome (data summary view –analytical method) ...........................................30 Figure 11. Laboratory means for lead in SRM 3398 Ginger (Zingiber officinale) Rhizome and SRM 3384 Ground Asian Ginseng (Panax ginseng C.A. Meyer) Rhizome (sample/sample comparison view) ..................................................................................31 s Figure 12. Laboratory means for total arsenic in SRM 3398 Ginger (Zingiber officinale) / /doi.org/10.6028/NIST.IR. Rhizome and SRM 3384 Ground Asian Ginseng (Panax ginseng C.A. Meyer) Rhizome (sample/sample comparison view) ..................................................................................32 WATER-SOLUBLE VITAMINS (B1, B2) IN DIETARY SUPPLEMENTS ...............................33 Study Overview .................................................................................................................33 Sample Information ...........................................................................................................33 Spirulina .................................................................................................................33 Multivitamin ...........................................................................................................33