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Dietary Supplement Laboratory Quality Assurance Program (DSQAP)

Summary

The National Institute of Standards and Technology (NIST), in collaboration with the National Institutes of Health (NIH) Office of Dietary Supplements (ODS), launched the Dietary Supplement Laboratory Quality Assurance Program (DSQAP) to support the measurement needs of the dietary supplements community. The DSQAP has provided an opportunity for dietary supplements testing laboratories to improve comparability of their measurements, as well as for NIST to assess community needs for reference materials, workshops, and other measurement services.

Description

Montage of photographs showing brewed green tea, filled capsules resting on a ginkgo leaf, seaweed, and ginsing roots, powder, and leaves.
Credit: Canva stock

Approximately 75% of the U.S. population takes dietary supplements, including vitamins and mineral supplements, representing an annual expenditure of more than $20 billion. Regulations, driven by reported cases of inaccurate labeling, adulteration, contamination (with pesticides, heavy metals, or toxic botanicals), and drug interactions, are now in place that require manufacturers to evaluate the identity, purity, and composition of their ingredients and finished products. In 2007, a Dietary Supplement Laboratory Quality Assurance Program (DSQAP) was initiated to enable participants to improve the accuracy and precision of their measurements for nutrients, marker compounds, toxic elements, and/or pesticides in dietary supplement ingredients and finished products. From 2017 to 2021, the participants of the DSQAP were served by studies conducted as part of the Health Assessment Measurements QAP. As part of a revamp of the NIST QAPs in 2021, NIST and ODS revitalized the DSQAP, which conducted its sixteenth exercise in 2022. In 2025, the DSQAP Consortium was launched to formalize the collaborative nature of the DSQAP efforts.

Approximately twice a year, exercises have offered participants the opportunity tomeasure concentrations of nutritional and toxic elements, fat- and water-soluble vitamins, fatty acids, active and/or marker compounds, and contaminants in samples distributed by NIST. Participant data was compiled at NIST and analyzed for accuracy, precision, and concordance within the community. Reports and certificates of completion were sent to participants. Workshops and other presentations offered opportunities to discuss results, measurement challenges, and methodological advancements in the characterization of dietary supplements. The intercomparison exercises, data reports, and workshops were designed to provide participating laboratories with the tools to evaluate their dietary supplement analytical methodology. Information gained through participation has been used by the participants to demonstrate "appropriateness" of analytical methodology to regulatory agencies and to improve the quality of information associated with dietary supplement products through increased measurement capabilities.

Future DSQAP studies will be conducted through the DSQAP Consortium and will be available to Consortium members only. 

PRE-CONSORTIUM EXERCISES AND OTHER MAJOR ACCOMPLISHMENTS

Pre-Consortium Exercises

Past participants can access historical results at QAP HUB. Log in using your existing credentials, or enter your email address to request a new password

Exercise 4 (2025)
StudyMeasurands and Samples
Nutritional ElementsCa, Cr, and Se in tablets and gummies
Water-Soluble Vitamins Vitamins B3 and B6 in tablets and gummies
BotanicalsAnthocyanidins in bilberry and cranberry extracts

Samples for Exercise 4 will ship in March 2025.

StudyMeasurands and Samples
Toxic ElementsAs, Cd, Pb, and Hg in kava root and kava extract
Fat-Soluble VitaminsVitamin A in multivitamin tablets
Water-Soluble VitaminsVitamins B1 and B2 in yohimbe containing solid oral dosage form and multivitamin tablets
BotanicalsKava lactones in kava root and kava extract

Exercise 3 Final Report is in progress

StudyMeasurands and Samples
Toxic ElementsAs, Cd, Pb, and Hg in eleuthero and ginger extracts
Fat-Soluble VitaminsTotal β-carotene in saw palmetto and multivitamin tablets
Botanicals IGingerols in ginger rhizome, extract, and ginger-containing supplements
Fatty AcidsFatty acids in fish oils
Botanicals IITriterpene glycosides in black cohosh rhizome and extract

Crossed out studies were offered but then cancelled due to low enrollment

Exercise 2 Final Report

StudyMeasurands and Samples
Elements*Ca, Cr, Mg, I, Na, K, As, Cd, Cu, Zn, Se, I, S, and Hg in kelp
Vitamins I*Vitamins B3 and K1 in kelp
Vitamins IIVitamins B1, B2, B3, B5, B6, B7, B9, & B12 in liquid and powdered drink mixes
Botanicals I*Phenolic content in kelp and green tea
Botanicals IIWithanolides in ashwagandha
Proximates*Ash, carbohydrates, fat, protein, solids, starch, total dietary fiber, and calories in kelp
Contaminants*PFAS in kelp

*Study run in part as a collaboration with World Wildlife Fund (WWF)
Exercise 1 Final Report

Dietary supplement related studies from 2017 to 2021 were conducted as part of the Health Assessment Measurements Quality Assurance Program (HAMQAP).

StudyMeasurands and Samples
Toxic ElementsAs, Cd, Pb, and Hg in black cohosh and turmeric
Natural ProductsCurcuminoids in turmeric; Chondroitin sulfate in supplements
BotanicalsBotanical ID: Ginkgo biloba

Exercise O Report

StudyMeasurands and Samples
Nutritional ElementsCr in a chromium supplement and multivitamin tablets
Toxic ElementsAs, Cd, and Pb in calcium supplement and ginkgo supplement
Water-Soluble VitaminsFolic acid in cereal and multivitamin tablets
Fat-Soluble Vitaminsvitamin D in protein powder, calcium supplement, and
multivitamin tablets
Fatty AcidsOmega-3 and -6 in saw palmetto berries and botanical oil
BotanicalsGinsenosides in ginseng

Exercise N Report

StudyMeasurands and Samples
Nutritional ElementsK and Zn in spinach and spirulina
Toxic ElementsAs and Pb in ginger and ginseng
Water-Soluble VitaminsVitamins B1 and B2 in spirulina and multivitamin tablets
Fat-Soluble VitaminsVitamin K1 in basil and kelp
BotanicalsCurcuminoids in turmeric
IdentityChondroitin sulfate

Exercise M Report

StudyMeasurands and Samples
Nutritional ElementsIodine in cat food and multivitamin tablets
Toxic ElementsAs and Pb in St. John’s wort
Water-Soluble VitaminsBiotin in cat food and multivitamin tablets
Fat-Soluble VitaminsLutein and zeaxanthin in spinach and multivitamin tablets
Fatty AcidsOmega-3 and -6 in fish oils
BotanicalsChlorogenic acid, flavonoids, and naphthodianthrones in St. John’s wort

Exercise L Report

StudyMeasurands and Samples
Nutritional ElementsP and Fe in cranberry and blueberry
Toxic ElementsHg in Ephedra and Ginkgo
Water-Soluble VitaminsVitamins B1, B2, and B3 in multivitamin tablets and protein powder
Fat-Soluble VitaminsVitamin K1 in multivitamin tablets and protein powder
ContaminantsAcrylamide in chocolate and coffee
BotanicalsPhytosterols in saw palmetto

Exercise K Report

StudyMeasurands and Samples
Nutritional ElementsCa, Mg, and Z in natural and enhanced waters
Toxic ElementsAs in St. John's wort
Water-Soluble VitaminsVitamins B1, B3, and B6 in multivitamin tablets and enhanced water
Fat-Soluble VitaminsVitamin E in multivitamin tablets and enhanced water
Fatty AcidsOmega-3 and -6 fatty acids in plant and fish oils
ContaminantsAflatoxins in peanut products
BotanicalsIsoflavones in soy protein isolate and soy flour
IdentityPure and adulterated Ginkgo biloba.
**Consensus-based only, no quantitative results required

Exercise J Report

StudyMeasurands and Samples
Nutritional ElementsCr, Mo, and Se in egg powder and multivitamin tablets
Toxic ElementsCd in breakfast cereal and calcium supplement
Water-Soluble VitaminsPantothenic acid soy flour and blueberries
Fat-Soluble VitaminsVitamin A in egg powder and breakfast cereal
BotanicalsCatechins in green tea leaves and extract

Exercise I Report

StudyMeasurands and Samples
Nutritional ElementsCa, Cu, and Mn in calcium supplement and oyster tissue
Water-Soluble VitaminsCholine in soy flour and egg powder
Fat-Soluble VitaminsTocopherols in carrot oil and egg powder
Fatty AcidsOmega-3 and -6 fatty acids in saw palmetto extract and berries
ContaminantsPAHs in neat solution and green tea leaves
BotanicalsPhytosterols in flax and perilla oils

Exercise H Report

StudyMeasurands and Samples
Nutritional ElementsNa in tomato leaves and cranberry powder
Toxic ElementsPb in multivitamin tablets and Ephedra-containing tablets
Water-Soluble VitaminsFolate in breakfast cereal and fortified milk powder
Fat-Soluble Vitaminsβ-carotene in ethanolic solutions and saw palmetto extract
BotanicalsAnthocyanins/anthocyanidins in cranberry and bilberry extracts

Exercise G Report

Exercise F (2010-2011)

StudyMeasurands and Samples
Nutritional ElementsNa and Fe in chocolate, spinach, and blueberries
Toxic ElementsAs, Cd, Pb, and Hg in green tea
Water-Soluble VitaminsVitamins B1, B3, B6, & B12 in milk powder, blueberries,
and B-vitamin tablets
Fat-Soluble VitaminsVitamin D in infant formula and supplements
Fatty AcidsFatty acids in botanical oils, fish oils, and fish tissue
BotanicalsIsoflavones in soy-containing products

Participants in DSQAP Exercise F can request a copy of the final report via email to QAPHUB [at] nist.gov (QAPHUB[at]nist[dot]gov).

StudyMeasurands and Samples
Nutritional ElementsCa, Fe, and Zn in fortified breakfast cereals
Water-Soluble VitaminsNiacin in fortified breakfast cereals
Fat-Soluble Vitaminsβ-carotene in oil and multivitamin tablet
ContaminantsAflatoxins in peanut products
BotanicalsCatechins in green tea

Exercise E Report

StudyMeasurands and Samples
Toxic ElementsPb in Ginkgo
Water-Soluble VitaminsNiacin in fortified milk powder
Fat-Soluble Vitaminsβ-carotene in oils
BotanicalsOrganic acids in berry extracts

Exercise D Report

StudyMeasurands and Samples
Nutritional ElementsCa, Na, P, and Zn in protein drink mix and fortified milk powder
Toxic ElementsAs and Cd in bitter orange
Water-Soluble VitaminsNiacin and vitamin B6 in protein drink mix and fortified milk powder
Fat-Soluble VitaminsRetinyl palmitate in fortified milk powder
Fatty AcidsOmega-3 and omega-6 fatty acids in botanical oils
BotanicalsPhytosterols in a neat solution and saw palmetto

Exercise C Report

StudyMeasurands and Samples
Toxic ElementsAs in Ephedra
Water-Soluble VitaminsVitamins B1 & B2 in multivitamin tablets
BotanicalsPhytosterols in saw palmetto, flavonols in Ginkgo biloba
synephrine in bitter orange

Exercise B Report

StudyMeasurands and Samples
Nutritional ElementsCa, Fe, Mg, and Zn in multivitamin tablets
Toxic ElementsPb in Ginkgo and Ephedra tablets
Water-Soluble VitaminsFolic acid in multivitamin tablets and infant formula
Fat-Soluble VitaminsVitamins A & E in multivitamin tablets and infant formula
Fatty AcidsFatty acids in vegetable oil blends
BotanicalsCaffeine in solid oral dosage forms

Exercise A Report

Pre-Consortium Workshops

Supporting The Standardization of Seaweed Measurements Workshop (October 24, 2023): In support of the DSQAP Exercise 1 seaweed collaboration with World Wildlife Fund (WWF), NIST hosted a workshop to discuss the QAP results, observations, and technical recommendations, as well as provide opportunities for discussions on improving measurement capabilities. The workshop included presentations from both NIST staff and external experts, along with discussions between NIST staff and participants for more in-depth conversations. These discussions with the research and analytical laboratory communities included the importance of robust and validated analytical methods and the future role of NIST in supporting seaweed measurement standardization.

NIST DSQAP Workshop (April 23, 2023): NIST and the University of Mississippi National Center for Products Research co-sponsored a half-day workshop that was held in conjunction with the 21st Oxford International Conference on the Science of Botanicals (ICSB). The workshop described recent updates to NIST QAP offerings, and focused on discussion of the analytical challenges in measuring nutrients, phytochemicals, or contaminants in dietary supplements, botanicals, and other natural products.

RELATED REFERENCE MATERIALS

As part of a multi-year interagency agreement among the NIST, the NIH/ODS, the Food and Drug Administration (FDA) Center for Food Safety and Applied Nutrition (CFSAN), and the FDA Center for Drug Evaluation and Research (CDER), NIST is developing Reference Materials (RMs) and Standard Reference Materials (SRMs) for botanical dietary supplements. RMs and SRMs with assigned values for concentrations of active and/or marker compounds, pesticides, and toxic elements are being produced to assist in the verification of manufacturers' label claims and for use in quality control during the manufacturing process in support of the Good Manufacturing Practices released by the FDA in 2007. 

For the most up-to-date information about available RMs and SRMs, visit the NIST Store.

Associated Publications

If you or your institution subscribe to a journal cited below, clicking on the link should take you to a page from which you can access the reference.

Created December 17, 2008, Updated January 24, 2025