Statement of Work.docx

Statement of Work

The Dietary Supplement Ingredient Database: Monitoring Ingredient Levels and Performance Quality of Dietary Supplements on the U.S. Market

I. Background Information and Objectives

A. Background Information

One of the missions of the Methods and Application of Food Composition Laboratory (MAFCL) is to develop authoritative estimates of bioactive components and ingredients in foods and dietary supplements (DS) to support the development of USDA composition databases and state-of-the-art methods to acquire, evaluate, compile and disseminate composition data on foods and DS available in the United States.

Since 2004, the USDA has been gathering information about ingredients and bioactive components in DSs, based on chemical analysis. Composition data for foods and DS are needed to support research, policy development and dietary guidance concerning the availability of a safe, nutritious and adequate diet. These data are the basis of essentially all public and private work in the field of nutrition. Nutrition monitoring activities and their results depend heavily on food and DS composition data. The What We Eat in America (WWEIA) component of the National Health and Nutrition Examination Survey (NHANES) use these data to calculate ingredient intake and determine the adequacy of the diet for the U.S. population. The labeled ingredient levels in DS are incorporated into these intake calculations, increasing the need for validated data.

The Dietary Supplement Ingredient Database (DSID) was first launched in 2009 to provide an analytically based database which can be used as a research tool to more accurately measure the intake of nutrients and other bioactive ingredients in the U.S. The fourth version of the DSID, DSID-4 (https://dsid.usda.nih.gov), was released in 2017. It provides national estimates for ingredients content in adult, children's and non-prescription prenatal multivitamins and for ingredients in omega-3 fatty acid DSs.

For the DSID project, MAFCL relies on contracts with commercial laboratories to test DS for ingredient content and performance quality.

B. Objectives

The purpose of this contract is to partner with laboratories to obtain accurate and representative analytical data for ingredients in DS and other tests of DS performance. These data will be obtained through physical tests and chemical assays by laboratories utilizing valid, up-to-date analytical methodology and rigorous quality control (QC) programs based on the use of Certified Reference Materials (CRMs), other in-house QC materials and thorough documentation.

II. Services to be performed

A. General Requirements

The Contractor shall test and analyze the DS samples sent to them by MAFCL or our designee. Attachment 1lists the tests to be performed and ingredients to be analyzed.

In the event additional testing or ingredient analyses are required, we may modify the contract to include them. The Contractor may be required to demonstrate expertise by submitting methods, validation information and control charts.

B. Specific Task/Technical Requirements Task 1. Ingredient Analyses and Tests

1.1 Homogenization and extraction of Dietary Supplement samples

Dietary supplement samples will be shipped in the units sold (as tablets, softgels, capsules, powders, chewable tablets, gummies, soft chews, liquids, etc.) and are likely to include a variety of ingredients. Most will require weighing, grinding and/or homogenization appropriate for the form of the supplement. Weights must be reported to four decimal places.

In the case of tablets and capsules, weights shall be determined by weighing at least 20 tablets or capsules before grinding/homogenization. For samples that are capsules, an additional weighing of the cleaned and dried hard or soft shells is necessary. All weights will be reported with the ingredient test results, along with the method and exact length of time of homogenization. For liquids, specific gravity must be determined.

Some samples may require additional steps or equipment, which could include moisture analysis, additional grinding of powdered samples, cryogenic grinding, etc. Unique homogenization procedures may be required for labile ingredients (e.g. folic acid, vitamin C, beta-carotene and other carotenoids). Special homogenization or extraction procedures may be required for DS with microencapsulated components and liquid emulsions/suspensions.

For chemical assays, the DS studies at MAFCL require homogenization of at least 20 tablets/capsules/units, unless both parties agree on a smaller number.

1.2 Primary Ingredient Analyses and Tests

Samples will be sent in batches of 20-30 samples. MAFCL sends blinded quality control samples (including certified reference materials, in house control materials and duplicate samples) as part of each batch of product samples, to monitor the accuracy and precision of the laboratory results.

The Contractor will be informed about samples to be sent at least a week before shipment, or earlier if preferred. Over the course of a year, batches of samples may be clustered together, with 3-

4 batches sent in a month (50-80 samples) and no samples sent for 2-3 months at a time. In most cases, more than one ingredient/constituent will be tested. The number of ingredients/constituents to be analyzed may be >20 (in the case of multivitamin/multimineral products). Most of the samples will be DS in forms sold to consumers, but occasionally raw materials will be tested.

Instructions will be provided in a cover letter for each set of samples, which will be emailed when the samples are shipped. MAFCL expects these instructions to be followed. If the Contractor has any questions about the instructions, they should request clarification before testing the samples.

Additional sample information will be provided in excel spreadsheets emailed along with the cover letter.

Upon receipt, samples are to be evaluated to determine whether all samples have been received and are in good condition. MAFCL is to be notified immediately in the event of any problems.

Samples are to be stored according to the instructions provided for that group of samples. Storage conditions may vary from -60°C to room temperature. Most samples will require a weighing step and a homogenization step. After homogenization, samples are to be stored at -60°C, unless they are being analyzed immediately or if the instructions specify otherwise. Samples are to be handled in such a way as to maintain sample integrity for the ingredient content, and to ensure homogeneity of aliquots used for analysis of specific ingredients. If special handling is required, instructions will be sent with the samples.

Samples shall be analyzed for the ingredients specified by MAFCL in the instructions accompanying the samples. All vitamins and other labile constituents in DS shall be analyzed within one day after preparing the homogenate. It is important to note that for chemical assays, the DS studies at MAFCL require at least 20 tablets/capsules to be homogenized. Aliquots from this homogenate should be used for the assays. If the DS to be tested are quite large (e.g., soft chews >5 g each), MAFCL may accept homogenization of <20 sample units.

The laboratory shall use methods approved by the Association of Official Analytical Chemists (AOAC, International), the United States Pharmacopeia (USP), or equivalent methods, including in-house methods which have been validated in your facility. Any modifications to the standard analytical methods shall be documented, and non-AOAC methods must be fully described. Appropriate quality control procedures shall also be employed during the analyses and reported to MAFCL. Results of analyses shall be reported in the units and to the number of significant figures specified in Attachment A. Unique homogenization procedures may be required for certain labile ingredients (e.g. folic acid, vitamin C, beta-carotene and other carotenoids). Special homogenization or extraction procedures may be required for DS with microencapsulated components and liquid emulsions/suspensions.

If during the contract period, the Contractor wishes to change a method specified in their proposal, they may do so after providing validation for the new or modified method and after acceptance by the Contracting Officer's Representative (COR).

The remainder of the homogenized samples shall be stored at -60° C (or as specified) until the results are approved and the study is completed. The Contractor must get permission from the DS laboratory liaison to discard any stored test samples.

1.3 Repeat Analyses and Tests

If MAFCL has questions about the test and assay results received, the Contractor will be contacted by email or phone. A conference call may be requested with the Contractor to review the results for MAFCL's quality control samples, the Contractor's provided QC information, the sample results, and to discuss in detail questions about sample handling, homogenization, extraction, testing and results.

It is likely that a number of samples will require retesting (repeat analyses or tests).

A. If retesting is required because of a failure by the Contractor to follow instructions for sampling handling (e.g., storage temperature or number of units to be homogenized) or to follow procedures for documented methods, the additional costs will be the Contractor's responsibility.

B. If retesting is required due to errors in dilution or calculations by the Contractor, the additional costs will be the Contractor's responsibility.

C. If retesting is needed to verify unusual results (e.g., 70% above or below label claims, or results atypical of most samples), MAFCL will be responsible for the additional testing costs.

Sample retests are handled in one of two ways:

· An additional 20 units of the sample (or appropriate weight of liquids or powders) will be sent with a new test sample ID.

· Frozen homogenates of the original samples stored by the Contractor may be used for retesting.

The Contractor shall have 30 days to respond to a request to repeat any tests or analyses and to resolve any questions.

The remainder of the homogenized samples shall be stored at -60° C (or as specified) until the results are approved and the study is completed. The Contractor must get permission from the DS laboratory liaison to discard any stored test samples.

Task 2. Reporting Requirements

The Contractor shall prepare reports as specified below. With each batch of samples sent, a reporting sheet (in excel format) is also sent. The Contractor is required to fill in the excel sheet with the sample results and email it to MAFCL.

2.1 Monthly Tracking Reports

In lieu of formal monthly reports, a tracking sheet is due once a month. The report shall be sent by email to the laboratory liaison and shall contain, for each Task Order:

· List of batches received and awaiting analysis, along with expected dates of completion

· List of batches with completed analyses and the date completed (a cumulative listing)

· Additional relevant information

2.2 Data Files Results

Data files reporting the results of analyses are due no more than 30 days after receipt of each batch of samples for analysis. The data file submission shall contain the following:

· A list of samples included in the data submission

· Detailed descriptions of sample processing, including any special procedures

· Methods of analysis, including any modifications

· The results of internal quality control procedures conducted at the same time as the analyses of the submitted samples

· Results for all analyses specified in the instructions accompanying a batch of samples in the units and the number of decimal places specified in Attachment 1 of the SOW;

· All sample weights and other sample information

· Sample density, if a liquid sample

· For DS physical testing, information about the appearance of the dosage forms may be required, along with visual documentation of dosage form and medium appearances at designated time points. We can provide USB thumb drives for large files.

Ingredient results and other data presented in each data file shall be delivered in Microsoft Excel spreadsheet format sent by e-mail. The columns required will be sent with the shipment information and will include at least:

1. Laboratory sample number

2. Sample number assigned by MAFCL

3. Sample description from the analysis request sent with the sample

4. Sample weight (for ingredient results)

5. Sample size in grams or mg (at least 3 significant figures)

6. Ingredient analyzed or test name

7. Ingredient form reported

8. Extraction method, if different from the normal method

9. Results (with at least 3 significant figures for ingredient results)

10. Units

11. Indication if value is less than the LOD/LOQ and a listing of these quantities

12. Date of analysis

13. For disintegration and dissolution tests, MAFCL checklists shall be filled out and sent to MAFCL along with the results

A separate file shall be created for each batch of samples. The Contractor's QC results shall be reported on a separate tab and include the name of the control material, ingredient analyzed, sample matrix, date of analysis, analytical result, and target values and ranges.

Any change in data format submissions shall be clearly defined and agreed upon by MAFCL.

The e-mail files shall not contain any copy-protection coding or formatting which would prevent the government from making additional copies of the files. THE DATA GENERATED BECOMES THE PROPERTY OF USDA AND SHALL NOT BE DISSEMINATED OR USED IN ANY OTHER WAY BY THE CONTRACTOR WITHOUT PERMISSION.

2.3 Problem Resolution Report

In the event a method or laboratory performance problem occurs, a report showing resolution of the problem will be due within 10 business days of request. The report shall contain the results of the analyses of the samples and steps taken to resolve the problem.