22 Jan 2021

Melamine Analysis for FDA Detention

When food products are imported into the United States, they can be detained by the Food and Drug Administration (FDA) if they are considered potentially unsafe and/or adulterated. Some examples include unacceptable range of protein assessed by Total Kjeldahl nitrogen (TKN) method, melamine with too high of percentage of nitrogen, health risks for infants/animals, or melamine being identified in protein isolates. Whatever the reason, these products may need analytical testing to prove they meet US regulatory requirements and are safe for consumption before being released from detention and entering the market. Melamine analysis can play an important role in assessing the food and getting it released and into the US marketplace.

Document Collection/Review

The first step to getting products released from the FDA is documentation. First, it is important to verify the product to be inspected, including information on the shipment to be sampled. From this, you will develop a sampling plan for the detained shipment, which you should outline. Documentation should also include information from the supplier's certificates of analysis: the manufacturer's factory location, product lot number, manufacturing dates and expiration dates. You will also need the shipping manifests, particularly lot numbers, quantity of pallets, container sizes and a sampling plan based off this information. Finally, you will need a bill of lading identifying the total shipment weight, port of entry and country of origin.


To run an analysis, samples are collected in accordance with FDA regulations. The sampling must be representative and include sublots. Sample points are selected at random from the middle of the pallets at a rate of 500-gram portions/sublot). Markings and/or labels are photographed. Then, samples are labeled, double bagged, and sealed with a unique seal number to prevent breakage and contamination during transportation. All sample and seal numbers are recorded on a chain of custody and submitted to the laboratory for further analysis.

In the lab, samples are received, and the chain of custody is documented. The lab then randomly selects samples for analysis. The number of samples used for analysis will be determined by the square root of the number of containers, but no less than 12 and no more than 36 samples per lot can be assessed. Duplicate portions from each sample are used.

The method of development and validation must comply with FDA required methodology. The method is validated at the lab and all future submissions must follow the validated method. Analysis of Melamine and Cyanuric Acid is required and can be determined using LC-MS-MS techniques. The detection limit of each compound must be less than or equal to 0.25 parts per million (ppm).

The sample is prepared, as is the standard and a solvent blank is used for quality control. Data is collected and pulled into a report. All the raw data and documentation is submitted directly to the FDA, along with the resume of the chemist who performed the analyst. Each page of the report is initialed and dated and the package is electronically uploaded to the agency who then reviews it and updated the status online.

It is important to move quickly with a trusted partner to get products released from the limbo of FDA detention and into the market, particularly when shelf-life concerns are taken into consideration. Learn more about the process and Intertek's services in our webinar recording.



Kenneth Cote,
Director of Agriculture and of Food


Kenneth Cote, Director of Agriculture and of Food at Intertek, has been in the agricultural industry for more than 15 years, starting his career as a barge sampler and advancing to his current leadership role. He has worked with multiple cargos and situations around the world. Ken utilizes his experience working within the agricultural, fertilizers, foods, dietary supplements, metals, minerals, solid fuels, plastics, chemicals, veg oils and regulatory compliance industries to add value to our customers.

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