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1.  Progress in developing analytical and label-based dietary supplement databases at the NIH Office of Dietary Supplements 
Although an estimated 50% of adults in the United States consume dietary supplements, analytically substantiated data on their bioactive constituents are sparse. Several programs funded by the Office of Dietary Supplements (ODS) at the National Institutes of Health enhance dietary supplement database development and help to better describe the quantitative and qualitative contributions of dietary supplements to total dietary intakes. ODS, in collaboration with the United States Department of Agriculture, is developing a Dietary Supplement Ingredient Database (DSID) verified by chemical analysis. The products chosen initially for analytical verification are adult multivitamin-mineral supplements (MVMs). These products are widely used, analytical methods are available for determining key constituents, and a certified reference material is in development. Also MVMs have no standard scientific, regulatory, or marketplace definitions and have widely varying compositions, characteristics, and bioavailability. Furthermore, the extent to which actual amounts of vitamins and minerals in a product deviate from label values is not known. Ultimately, DSID will prove useful to professionals in permitting more accurate estimation of the contribution of dietary supplements to total dietary intakes of nutrients and better evaluation of the role of dietary supplements in promoting health and well-being. ODS is also collaborating with the National Center for Health Statistics to enhance the National Health and Nutrition Examination Survey dietary supplement label database. The newest ODS effort explores the feasibility and practicality of developing a database of all dietary supplement labels marketed in the US. This article describes these and supporting projects.
PMCID: PMC4208495  PMID: 25346570
Dietary supplements; Analytical substantiation; Dietary supplement composition; Dietary supplement ingredient database; NHANES; DSID; NHANES-DSLD; DSLD-USA; Dietary supplement labels; Standard reference materials®; Certified reference materials
2.  Progress in development of an integrated dietary supplement ingredient database at the NIH Office of Dietary Supplements 
Several activities of the Office of Dietary Supplements (ODS) at the National Institutes of Health involve enhancement of dietary supplement databases. These include an initiative with US Department of Agriculture to develop an analytically substantiated dietary supplement ingredient database (DSID) and collaboration with the National Center for Health Statistics to enhance the dietary supplement label database in the National Health and Nutrition Examination Survey (NHANES). The many challenges that must be dealt with in developing an analytically supported DSID include categorizing product types in the database, identifying nutrients, and other components of public health interest in these products and prioritizing which will be entered in the database first. Additional tasks include developing methods and reference materials for quantifying the constituents, finding qualified laboratories to measure the constituents, developing appropriate sample handling procedures, and finally developing representative sampling plans. Developing the NHANES dietary supplement label database has other challenges such as collecting information on dietary supplement use from NHANES respondents, constant updating and refining of information obtained, developing default values that can be used if the respondent cannot supply the exact supplement or strength that was consumed, and developing a publicly available label database. Federal partners and the research community are assisting in making an analytically supported dietary supplement database a reality.
PMCID: PMC4191662  PMID: 25309034
Dietary supplements; Analytical substantiation; Dietary supplement composition; Dietary supplement ingredient database; NHANES; DSID; Dietary supplement labels; Certified reference materials; Standard reference materials
3.  Accuracy, Precision, and Reliability of Chemical Measurements in Natural Products Research 
Fitoterapia  2010;82(1):44-52.
Natural products chemistry is the discipline that lies at the heart of modern pharmacognosy. The field encompasses qualitative and quantitative analytical tools that range from spectroscopy and spectrometry to chromatography. Among other things, modern research on crude botanicals is engaged in the discovery of the phytochemical constituents necessary for therapeutic efficacy, including the synergistic effects of components of complex mixtures in the botanical matrix. In the phytomedicine field, these botanicals and their contained mixtures are considered the active pharmaceutical ingredient (API), and pharmacognosists are increasingly called upon to supplement their molecular discovery work by assisting in the development and utilization of analytical tools for assessing the quality and safety of these products. Unlike single-chemical entity APIs, botanical raw materials and their derived products are highly variable because their chemistry and morphology depend on the genotypic and phenotypic variation, geographical origin and weather exposure, harvesting practices, and processing conditions of the source material. Unless controlled, this inherent variability in the raw material stream can result in inconsistent finished products that are under-potent, over-potent, and/or contaminated. Over the decades, natural products chemists have routinely developed quantitative analytical methods for phytochemicals of interest. Quantitative methods for the determination of product quality bear the weight of regulatory scrutiny. These methods must be accurate, precise, and reproducible. Accordingly, this review discusses the principles of accuracy (relationship between experimental and true value), precision (distribution of data values), and reliability in the quantitation of phytochemicals in natural products.
PMCID: PMC3026088  PMID: 20884340
Accuracy; Precision; Validation; Analytical Methods; Natural Products; Herbals
4.  Dietary supplement ingredient database (DSID): Preliminary USDA studies on the composition of adult multivitamin/mineral supplements☆ 
The Nutrient Data Laboratory of the United States Department of Agriculture (USDA) is collaborating with the Office of Dietary Supplements (ODS), the National Center for Health Statistics (NCHS), and other government agencies to design and populate a dietary supplement ingredient database (DSID). This analytically based, publicly available database will provide reliable estimates of vitamin and mineral content of dietary supplement (DS) products. The DSID will initially be populated with multivitamin/mineral (MVM) products because they are the most commonly consumed supplements. Challenges associated with the analysis of MVMs were identified and investigated. A pilot study addressing the identification of appropriate analytical methods, sample preparation protocols, and experienced laboratories for the analysis of 12 vitamins and 11 minerals in adult MVM supplement products was completed. Preliminary studies support the development of additional analytical studies with results that can be applied to the DSID. Total intakes from foods and supplements are needed to evaluate the associations between dietary components and health. The DSID will provide better estimates of actual nutrient intake from supplements than databases that rely on label values alone.
PMCID: PMC3846171  PMID: 24307755
Dietary supplements; Analytical database; DSID; Multivitamin; Pilot study; Nutrients
5.  Dehydropyrrolizidine Alkaloids, Including Monoesters with an Unusual Esterifying Acid, from Cultivated Crotalaria juncea (Sunn Hemp cv.’Tropic Sun’) 
Cultivation of Crotalaria juncea L. (Sunn Hemp cv. ‘Tropic Sun’) is recommended as a green manure crop in a rotation cycle to improve soil condition, help control erosion, suppress weeds and reduce soil nematodes. Because C. juncea belongs to a genus that is known for the production of toxic dehydropyrrolizidine alkaloids, extracts of the roots, stems, leaves and seeds of ‘Tropic Sun’ were analyzed for their presence using HPLC-ESI/MS. Qualitative analysis identified previously unknown alkaloids as major components along with the expected macrocyclic dehydropyrrolizidine alkaloid diesters, junceine and trichodesmine. The dehydropyrrolizidine alkaloids occurred mainly as the N-oxides in the roots, stems and, to a lesser extent, leaves, but mainly as the free bases in the seeds. Comprehensive spectrometric and spectroscopic analysis enabled elucidation of the unknown alkaloids as diastereoisomers of isohemijunceine, a monoester of retronecine with an unusual necic acid. The dehydropyrrolizidine alkaloid content of the roots, stems, leaves of immature plants was estimated to be 0.05, 0.12 and 0.01% w/w respectively while seeds were estimated to contain 0.15% w/w.
PMCID: PMC3366594  PMID: 22429238
Crotalaria juncea; ‘Tropic Sun’; pyrrolizidine alkaloids; N-oxides; HPLC-ESI/MS; junceine; trichodesmine; isohemijunceine; hemijunceine
6.  Determination of Major Phenolic Compounds in Echinacea spp. Raw Materials and Finished Products by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation Matrix Extension 
Journal of AOAC International  2011;94(5):1400-1410.
A method previously validated to determine caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid in echinacea raw materials has been successfully applied to dry extract and liquid tincture products in response to North American consumer needs. Single-laboratory validation was used to assess the repeatability, accuracy, selectivity, LOD, LOQ, analyte stability (ruggedness), and linearity of the method, with emphasis on finished products. Repeatability precision for each phenolic compound was between 1.04 and 5.65% RSD, with HorRat values between 0.30 and 1.39 for raw and dry extract finished products. HorRat values for tinctures were between 0.09 and 1.10. Accuracy of the method was determined through spike recovery studies. Recovery of each compound from raw material negative control (ginseng) was between 90 and 114%, while recovery from the finished product negative control (maltodextrin and magnesium stearate) was between 97 and 103%. A study was conducted to determine if cichoric acid, a major phenolic component of Echinacea purpurea (L.) Moench and E. angustifolia DC, degrades during sample preparation (extraction) and HPLC analysis. No significant degradation was observed over an extended testing period using the validated method.
PMCID: PMC3586990  PMID: 22165004
7.  Development and Certification of a Standard Reference Material for Vitamin D Metabolites in Human Seruma 
Analytical Chemistry  2011;84(2):956-962.
The National Institute of Standards and Technology (NIST), in collaboration with the National Institutes of Health’s Office of Dietary Supplements (NIH-ODS), has developed a Standard Reference Material (SRM) for the determination of 25-hydroxyvitamin D [25(OH)D] in serum. SRM 972 Vitamin D in Human Serum consists of four serum pools with different levels of vitamin D metabolites and has certified and reference values for 25(OH)D2, 25(OH)D3, and 3-epi-25(OH)D3. Value assignment of this SRM was accomplished using a combination of three isotope-dilution mass spectrometry approaches, with measurements performed at NIST and at the Centers for Disease Control and Prevention (CDC). Chromatographic resolution of the 3-epimer of 25(OH)D3 proved to be essential for accurate determination of the metabolites.
PMCID: PMC3287345  PMID: 22141317
8.  Effect of Increasing Doses of Saw Palmetto on Lower Urinary Tract Symptoms: A Randomized Trial 
Jama  2011;306(12):1344-1351.
Saw palmetto fruit extracts are widely used for treating lower urinary tract symptoms attributed to benign prostatic hyperplasia. However, recent clinical trials have questioned their efficacy, at least at standard doses (320 mg daily).
To determine the effect of a saw palmetto extract at up to three times the standard dose on lower urinary tract symptoms attributed to benign prostatic hyperplasia.
Multicenter placebo-controlled randomized trial conducted from June, 2008 through October, 2010.
Eleven North American clinical sites.
Were men at least 45 years old, with a peak urinary flow rate ≥ 4 ml/sec, an AUA Symptom Index (AUASI) score ≥ 8 and ≤ 24, and no exclusions.
One, two, and then three 320 mg daily doses of saw palmetto extract or placebo, with dose increases at 24 and 48 weeks.
Main Outcome Measures
Primary outcome was the difference in AUASI score from baseline to 72 weeks. Secondary outcomes were measures of urinary bother; nocturia; uroflow; postvoid residual; prostate-specific antigen; participants’ global assessments; and indices of sexual function, continence, sleep quality, and prostatitis symptoms.
From baseline to 72 weeks, mean AUASI scores decreased from 14.4 to 12.2 points with saw palmetto and from 14.7 to 11.7 points with placebo. The group mean difference in AUASI score change from baseline to 72 weeks between the saw palmetto and placebo groups was 0.79 points favoring placebo (bound of the 95% confidence interval most favorable to saw palmetto was 1.77 points, one-sided P=0.91). Saw palmetto was no more effective than placebo for any secondary outcome. No attributable side effects were identified.
Increasing doses of a saw palmetto fruit extract did not reduce lower urinary tract symptoms more than placebo. (CAMUS study number NCT00603304
PMCID: PMC3326341  PMID: 21954478
10.  Determination of Synephrine in Bitter Orange Raw Materials, Extracts, and Dietary Supplements by Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation 
Journal of AOAC International  2007;90(1):68-81.
A method has been developed to quantify synephrine in bitter orange raw material, extracts, and dietary supplements. Single-laboratory validation has been performed on the method to determine the repeatability, accuracy, selectivity, limit of detection/limit of quantification (LOQ), ruggedness, and linearity for p-synephrine and 5 other biogenic amines: octopamine, phenylephrine (m-synephrine), tyramine, N-methyltyramine, and hordenine, which may be present in bitter orange. p-Synephrine was found to be the primary biogenic amine present in all materials tested, accounting for >80% of the total biogenic amine content in all samples except a finished product. Repeatability precision for synephrine was between 1.48 and 3.55% RSD. Synephrine recovery was between 97.5 and 104%. The minor alkaloids were typically near the LOQ of the method (300–900 μg/g) in the test materials, and between-day precision for the minor compounds was poor because interferences could sometimes be mistakenly identified as one of the minor analytes. Recoveries of the minor components ranged from 99.1 to 103% at approximately 6000 μg/g spike level, to 90.7 to 120% at 300 μg/g spike level.
PMCID: PMC3207213  PMID: 17373438
11.  Dietary Supplement Laboratory Quality Assurance Program: The First Five Exercises 
Journal of AOAC International  2011;94(3):803-814.
The National Institute of Standards and Technology (NIST) has established a Dietary Supplement Laboratory Quality Assurance Program (DSQAP) in collaboration with the National Institutes of Health Office of Dietary Supplements. Program participants measure concentrations of active and/or marker compounds as well as nutritional and toxic elements in food and dietary supplements distributed by NIST. Data are compiled at NIST, where they are analyzed for accuracy relative to reference values and concordance among the participants. Performance reports and certificates of completion are provided to participants, which can be used to demonstrate compliance with current Good Manufacturing Practices as promulgated by the U.S. Food and Drug Administration. The DSQAP has conducted five exercises to date, with total participation including more than 75 different laboratories and many more individual analysts.
PMCID: PMC3173719  PMID: 21797008
12.  Determination of Aflatoxins B1, B2, G1, and G2 and Ochratoxin A in Ginseng and Ginger by Multitoxin Immunoaffinity Column Cleanup and Liquid Chromatographic Quantitation: Collaborative Study 
Journal of AOAC International  2008;91(3):511-523.
The accuracy, repeatability, and reproducibility characteristics of a method using multitoxin immunoaffinity column cleanup with liquid chromatography (LC) for determination of aflatoxins (AF; sum of aflatoxins B1, B2, G1, and G2) and ochratoxin A (OTA) in powdered ginseng and ginger have been established in a collaborative study involving 13 laboratories from 7 countries. Blind duplicate samples of blank, spiked (AF and OTA added) at levels ranging from 0.25 to 16.0 μg/kg for AF and 0.25 to 8.0 μg/kg for OTA were analyzed. A naturally contaminated powdered ginger sample was also included. Test samples were extracted with methanol and 0.5% aqueous sodium hydrogen carbonate solution (700 + 300, v/v). The extract was centrifuged, diluted with phosphate buffer (PB), filtered, and applied to an immunoaffinity column containing antibodies specific for AF and OTA. After washing the column with water, the toxins were eluted from the column with methanol, and quantified by high-performance LC with fluorescence detection. Average recoveries of AF from ginseng and ginger ranged from 70 to 87% (at spiking levels ranging from 2 to 16 μg/kg), and of OTA, from 86 to 113% (at spiking levels ranging from 1 to 8 μg/kg). Relative standard deviations for within-laboratory repeatability (RSDr) ranged from 2.6 to 8.3% for AF, and from 2.5 to 10.7% for OTA. Relative standard deviations for between-laboratory reproducibility (RSDR) ranged from 5.7 to 28.6% for AF, and from 5.5 to 10.7% for OTA. HorRat values were ≤2 for the multi-analytes in the 2 matrixes.
PMCID: PMC2586123  PMID: 18567295

Results 1-12 (12)