Although the Food Safety Modernization Act (FSMA) was signed into law in January 2011, revisions to many of the regulations delayed their implementation. Recently, the FDA established several of the final rules for compliance and activated them in August and October 2015. These include preventive controls for human food and animal feed, produce safety, Foreign Supplier Verification Program (FSVP), and third-party accreditation and certification. Compliance with the regulations is required within 18 months to two and a half years depending on the specific regulation. But what do FDA auditors really expect to see when they visit your business?
The FDA’s primary concern is ensuring that companies are following the regulations and therefore sends auditors to inspect the compliance records that companies keep, or may soon have to start keeping. The records demonstrate that the requisite steps were taken to meet compliance with the regulations. With regard to identification of contaminants, some food manufacturers may have to significantly augment their practices. Specifically, greater use of forensic or investigational analysis will be required. For example, food companies that obtain any portion of their product from outside of the U.S., whether whole or ingredients, will be subject to FSVP regulations. FSVP regulations require companies to investigate the origin of contaminants that may occur in their product. Under FSVP, the FDA will want to see the records for all stages of testing, including establishing the origin of contaminants. Although bulk analyses are great at establishing the presence of contaminants, bulk methods are not particularly good at identifying the what, when, and where of contamination; answering these questions typically requires forensic or investigational analysis methods. Maintaining the records from all stages of the investigation is vital for a successful positive outcome FDA audit.
Investigational Analysis: A New Paradigm
In the past, investigational analysis was not usually necessary in the food industry; the accepted norm was that most food ingredients were generally recognized as safe (GRAS). Establishing the provenance of contaminants can be costly, so firms typically limited investigational or forensic analysis to special cases, such as spices, where the product consists of a single, relatively high-priced ingredient, making the cost of analysis worthwhile. Alternatively, for some foods like spices, it was cheaper for large companies to simply buy or deal with source suppliers directly, removing middlemen and any incentive for economically motivated adulteration. However, the entire product processing path presents opportunities for contamination; both intentional and unintentional.
Enactment of FSMA and especially the FSVP now requires the food industry to provide more assurance and ultimately conduct more testing. The objective is no longer to simply identify contaminants but to understand and document how they ended up in the product. Additionally, records need to indicate and document who conducted the work during all stages of the identification.
To minimize the possibility of bias, the investigational analyses are best conducted, or corroborated, by an independent laboratory. The pharmaceutical industry has been subject to these types of regulations for years. This paradigm, although new to the food industry, brings positive advantages. For example, investigational analysis can provide greater confidence for establishing that a GRAS ingredient is safe even though a contaminant might be present. A food processor can remove certain contaminants, or prevent further contamination, once it understands how the contaminants manifest themselves in the product. Investigative analysis provides the pieces to the forensic contamination puzzle.
Investigational Analysis and Multiple Microscopy Methods
Any instance of product contamination or product failure can be traced to discreet particles or residues that may not be clearly visible or discernable to the naked eye. The size of contaminant particles can range from millimeters down to nanometers. Bulk analytical methods may identify the presence of a contaminant at trace or ultra trace concentrations, however they may not be of much use in identifying how that element came to be part of the product. Isolating the contaminants from the host product, on the other hand, allows for successful identification of the contaminants.
Isolating contaminant particulate begins with the use of an optical stereo zoom microscope. Visual inspection of an adulterated sample, in comparison to a reference sample, usually reveals a great deal about the contaminant, especially if it is particulate in nature. For example, metal contamination may occur as large pieces easily visible to the unaided eye, or as gray, brown, or orange (and sometimes green) spots in the product. The contaminant material can be isolated from the product under magnification using custom tools for handling microscopic size samples. A microscopic subsample can then be mounted on a suitable substrate for further analyses and identification. Continuing with the metal particulate example, inspection of the discolored samples with scanning electron microscopy (SEM) and X-ray microanalysis using an energy or wavelength dispersive spectrometer system (EDS or WDS), may reveal that the discolored areas contain micrometer sized particles of metal, even gauging the extent to which they have oxidized. X-ray microanalysis can establish the alloy type, allowing the manufacturer to narrow the search based on the product’s exposure to machinery composed of different alloys. This method of isolation and analysis is so powerful that sometimes the source of contamination can be traced to non-standard replacement parts installed by unqualified repair technicians.
In instances where polymers or other organic compounds are the contaminants, isolating these particles and pressing them out onto potassium bromide crystals for microscopy-based infrared spectroscopy yields amazing identification success.
When additional information is required, other methods provide a wide range of information about the nature of the particulate. These methods include micro X-ray diffraction, Raman microspectroscopy, transmission electron microscopy, electron spectroscopy for chemical analysis, and some mass spectrometry methods geared toward surface analysis.
Once particulate contaminants are isolated and fully characterized with multiple microscopy-based methods, it is generally easier to deduce how the contaminants came to be in the sample. This knowledge allows the product producer to correct the contamination issue at its source.
Collaborating with a Forensic Laboratory
Manufacturers and producers have a couple options when it comes to addressing their FSMA contamination identification requirements. The first is to construct an in-house laboratory capable of meeting the requirements in terms of competency, training and accreditation. The second is to utilize the services of third-party laboratories that are already accredited and ready to meet the quality requirements necessary for successful scrutiny by the FDA. Although many U.S. contract laboratories advertise compliance to current Good Manufacturing Practices (cGMP), a growing number of companies are operating at a global level and, therefore, need facilities that meet global standards. As such, meeting ISO standards is becoming a widely accepted and recognized quality program. ISO/IEC 17025:2005 covers the general requirements for the competence of testing and calibration laboratories, which includes elements beyond cGMP requirements. For ISO accreditation, a laboratory develops their quality program and then becomes accredited after inspection and approval by an ISO-recognized inspection company. With this system, manufacturers and producers can easily select an accredited laboratory to conduct their contaminant analysis and rest assured that the samples were analyzed using methods meeting the globally recognized ISO quality standard.
FSMA mandates more stringent measures to identify food product contaminants and their sources, established through testing. Forensic or investigational analysis has a recognized history of successfully helping the pharmaceutical industry meet similar FDA requirements for contamination. Many contaminants are actually particulate-scale materials that can be easily identified and their origin subsequently established using multiple microscopy methods. When contamination is an issue, using an ISO 17025 accredited laboratory can simplify meeting the full FSMA requirements.
Dr. Schwandt is a senior research scientist and director of industrial services at McCrone Associates, Inc., and co-teaches several courses at Hooke College of Applied Sciences, LLC, Westmont, Ill. Reach him at firstname.lastname@example.org.