Tag Archives: adulteration

FSMA Intentional Adulteration Rule Released

By Food Safety Tech Staff
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–UPDATE (5/27/2016)– The final rule has been published on the Federal Register‘s website. –END UPDATE–

FDA just released the final FSMA rule, “Mitigation Strategies to Protect Food Against Intentional Adulteration”. Under the rule, domestic and foreign food facilities must complete and maintain a written food defense plan that assesses their vulnerabilities to intentional contamination.

“Today’s final rule on intentional adulteration will further strengthen the safety of an increasingly global and complex food supply,” said Stephen Ostroff, M.D., incoming FDA deputy commissioner for foods and veterinary medicine in a press release. “The rule will work in concert with other components of FSMA by preventing food safety problems before they occur.”

The final rule will be published on the Federal Register tomorrow. To preview the PDF document, visit the Federal Register’s website.

FDA

FDA’s Annual Food Registry Report Finds Listeria and Allergens as Top Issues

By Food Safety Tech Staff
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FDA

Yesterday FDA released its Reportable Food Registry (RFR) and cited Listeria monocytogenes as generating the greatest number of reports (223), along with undeclared milk (27), in Year Five (from September 8, 2013–September 7, 2014).

FDA defines a reportable food as “an article of food/feed for which there is a reasonable probability that the use of, or exposure to, such article of food will cause serious adverse health consequences or death to humans or animals.” The purpose of the registry is to allow FDA to track patterns of food and feed adulteration in order to help the agency focus its already limited inspection resources.

Year Five saw 909 reportable food entries, including 201 primary reports regarding safety concerns with food or animal feed and 464 subsequent reports from suppliers or recipients of food or feed that was the subject of the primary reports, and 244 amended reports. The following food safety hazards were identified within the 201 primary reports in Year Five: Drug contamination, pathogenic E. coli, Listeria monocytogenes, nutrient imbalance, lead, Salmonella, undeclared allergens and undeclared sulfites. In addition, Salmonella, Listeria and undeclared allergens made up about 88% of the total primary entries for all five years of the RFR.

The report’s complete breakdown of the RFR submissions by year, along with identified commodities and hazards, is available on FDA’s website.

Department of Justice seal

Watch Out, DOJ and FDA Prioritizing Prosecution

By Food Safety Tech Staff
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Department of Justice seal

In remarks made at the Consumer Federation of America’s annual food policy conference this week, Benjamin C. Mizer, principal deputy assistant attorney general, stated that the federal government has made consumer safety a top priority. With this announcement comes an announced intention on the part of the U.S. Department of Justice (DOJ) to use “various enforcement tools that we have at our disposal,” and maintain a stronger partnership with FDA to go after companies that “introduce adulterated foods into interstate commerce”.

“In deciding whether to use our civil or our criminal enforcement tools, the Justice Department follows the same set of guidelines that apply to every criminal prosecution,” said Mizer. “Among other things, prosecutors evaluate the nature and seriousness of the offense, the deterrent effect of the prosecution and the culpability of the individuals or entities involved.” Criminal charges brought against a food company can be either misdemeanor or felony, and Mizer emphasized that misdemeanor violations can still result in “serious penalties”. He cited a case in which the owner and CEO of an egg production company in Iowa pled guilty to a misdemeanor and received three months in jail and one year supervised release, and was slapped with a $100,000 fine.

“In some cases, the facts are so egregious that it is appropriate for the Justice Department to bring the full force of the law to bear,” stated Mizer. “When we can show an intent to defraud or to mislead consumers or the FDA, a defendant can face felony charges.” To illustrate this scenario, Mizer referred to the landmark case against the Peanut Corporation of America, which is perhaps the most commonly referenced case in recent months, as many in the industry have voiced their opinion that it has set a precedent as to how the government will handle such situations moving forward.

Federal Government Takes Regulatory and Criminal Offensive Against Food Industry

 

Food Fraud

Fertilizer-Tainted Sugar, Formalin-Drenched Chicken Guts Top Fake Foods List

By Food Safety Tech Staff
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Food Fraud

–Update– 4/1/2016 16:40 pm–

This article was part of our April Fool’s special edition. While the information about the Interpol seizure is indeed factual, we made up the new detection method (EFAS). 35% of poll participants were correct in guessing that this was the article that contained false information.

This week Interpol-Europol announced its largest-ever seizure of fake foods and beverages across 57 countries over a four-month time period. In total, Operation Opson V seized 10,000 tones and 1 million liters of food products between November 2015 and February 2016, with the following topping the list:

  • Fertilizer-contaminated sugar from Khartoum, Sudan (nearly 9 tons)
  • Olives painted with copper sulphate solutions to enhance color (85+ tons)

“Today’s rising food prices and the global nature of the food chain offer the opportunity for criminals to sell counterfeit and substandard food in a multi-billion criminal industry which can pose serious potential health risks to unsuspecting customers. The complexity and scale of this fraud means cooperation needs to happen across borders with a multi-agency approach,” said Chris Vansteenkiste, cluster manager of the Intellectual Property Crime Team at Europol in an agency release.

Other seized products worthy of note include:

  • Chicken intestines preserved in formalin from Indonesia (70 kg)
  • Monkey meat from Belgium
  • Locusts (11 kg) and caterpillars (20 kg) from France
  • Fake whiskey from Zambia (1300 bottles)
  • Tilapia unfit for human consumption imported to Togo (24 tons)
  • Honey from Australia  (450 kg)

And for the false information:

At a recent conference for food laboratory professionals, Gavin Rosenberg, Ph.D., discussed an emerging analytical method that could be game changing in detecting adulterated products in the field. Using electrostatic fluorescence absorbance spectroscopy (EFAS), Rosenberg’s lab has been able to probe the chemical composition of products, from liquids to bulk and high-moisture foods, while simultaneously assessing concentration in products such as meat and even spices. The rapid and portable method is also highly sensitive and can provide trace detection of pathogens, dyes, antibiotics and pesticides within 60 seconds.

“While still in the research stage, EFAS has been utilized in several studies and has successfully been shown to detect contaminants as well as ingredients that are frequently added to adulterate food products,” said Rosenberg.  He indicated that his team will pursue initial applications of the product to identify adulteration of olive oil (nearly 70% of olive oil is adulterated or diluted) and ground beef, specifically in the European and Asian markets.

Contamination, Adulteration Remain Highest Priority

By Maria Fontanazza
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Increased media attention and consumer awareness of verifying ingredients, detecting allergens and effectively tracing the source of outbreaks has placed much higher scrutiny on food processors and manufacturers. With the anticipated FSMA final rule on intention adulteration (Focused Mitigation Strategies to Product Food Against Intentional Adulteration) expected in late spring, having the ability to effectively detect and address product contamination and adulteration will be of significant importance to manufacturers. In preparation for the upcoming Food Labs Conference March 7–8, Food Safety Tech sat down with Craig Schwandt, Ph.D., director of industrial services at McCrone Associates, to learn how contamination is currently affecting food companies and what they should be doing to protect their products and ensure consumer safety.

Craig Schwandt will be presenting “Contaminant Particle Identification: Establishing Provenance and Complying with FSMA” at this year’s Food Labs Conference | March 7–8 | LEARN MOREFood Safety Tech: What are the big issues facing the food industry related to product contamination?

Craig Schwandt: I think the biggest issue facing the food safety industry is realizing that FSMA, in its final ruling, comes with requirements to ensure food safety from farm to table. In the past, many [ingredients] were GRAs, or generally recognized as safe, so when there was a contaminant, [food companies] had a lot of liberty in disposing of the batch and weren’t too concerned about where it came from.

FSMA is going to require that [food companies] keep records of what contaminants are found, how they address it and whether it’s a recurring problem, and [that they] have a procedure in place to track back and [conduct] forensic analysis. In the analytical services industry we call it investigational analysis, which is a description of what actually takes place for ascertaining what the contaminant is and how it got there. That information is provided to clients so they can track back in their production process—all the way to the raw materials and then ascertain where the contaminants came from in that production chain.

The big challenge will be in recognizing that they have to start keeping records and then actually doing the investigation to determine what contaminants are there and determine where they’re coming in.

Craig Schwandt_McCrone Associates
Craig Schwandt, Ph.D., McCrone Associates

FST: Are companies taking the right steps to detect and identify contaminants in food?

Schwandt: Some of them do and some don’t.  At last year’s Institute of Food Technologist’s conference in Chicago, there was a session on FSMA in which there were representatives from FDA, the Grocery Manufacturers Association and a major food company.  I was a little bit shocked by the food company’s position.  They felt they didn’t need to take all of the steps required by FSMA because they dealt directly with producers from all over the world.  They felt removing intermediaries from their supply chain sufficiently protected their products from adulteration. This seems to be oversimplifying the production and supply chain process. Even though they may directly deal with farmers, there’s still opportunity from the time food stuff is harvested to being dried, placed in containers, and shipped from overseas to the U.S.—there are several steps where unintentional contaminants can arise. So to say they didn’t need to look at the potential for contamination because they dealt directly [with farmers] is a bit oversimplified.  I think this perspective typifies some of the industry’s viewpoint at the moment.

The Foreign Supplier Verification Program specifically addresses this concern.  Even companies that deal directly with producers and supplies in the country of the product’s origin will be required to demonstrate that they tested it and verified it as uncontaminated.

The understanding and recognition by suppliers of these new regulations is the biggest issue facing the food industry right now—especially now that the final rulings have been issued and we’re in the grace period before compliance with the regulation is required.

FST: What technologies are helping in the effort to fight product adulteration, especially as it relates to FSMA compliance?

Schwandt: Handheld instrumentation is making headway at identifying, at a gross scale, screening capabilities—handheld x-ray fluorescence instrumentation and handheld infrared spectroscopy, to identify things at the bulk level. Mass spectrometry methods and chromatography are exceptional at their ability to do really fast general screening for chemical adulterants. I think many of the food laboratories and food companies have in-house laboratories and screen in that general way.

In terms of some of the solid phase contaminants, I think there’s a lack of in-house capability at the moment where one can use simpler [methods] like optical microscopy and another microscopy-based methods to identify the physical solid phase contaminants.

A good example is the use of magnetometers.  Many companies use large-scale process line magnetometers to highlight the presence of metal pieces in their product. A magnetometer tells you that there are metal contaminants in your product, it does not provide a specific alloy identification.  Whether one needs to go further to use additional methods and actually ascertain the composition of the alloy, is the question.  That’s a new requirement—to identify what it is and then to try and assess where in the process it may have occurred. Using a microscopy-based method is advantageous because metal pieces are easily isolated and identified. Once food industry clients have an idea of what the alloy is, they can compare it to the metal alloys that make up their machinery along the way, whether it’s packaging or sorting machinery, [and] essentially establish where the particles enter into the food process.

Next-Generation DNA Sequencing Finds Unexpected Contaminants

By Food Safety Tech Staff
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With more regulatory and consumer scrutiny being placed on the authenticity of food products, companies must use technologies that can verify products and ingredients, and detect contaminants. NSF International recently acquired AuthenTechnologies, a testing laboratory that provides DNA-species identification services to improve authenticity, safety and quality of natural products. Using shorter segments and validated reference materials, AuthenTechnologies employs a DNA sequencing method that can identify “almost any” species and detect contaminants that cannot be distinguished morphologically or chemically. The method also screens for allergens, GMOs, fillers and filth.

“As the food supply chain becomes more complex and regulations continue to evolve and become more rigorous, this technology is becoming essential to achieving regulatory compliance and brand protection while preventing issues associated with fraud, mislabeling and adulteration,” said Lori Bestervelt, Ph.D, international executive vice president and chief technology officer at NSF, in a company release. AuthenTechnologies’ co-founder Danica Harbaugh Reynauld, Ph.D., adds, “We’ve developed a more highly specific DNA methodology capable of identifying a single organism to a complex blend of unlimited ingredients.” Reynauld, who will join NSF as global director of scientific innovation, will lead the NSF AuthenTechnologies center of excellence with NSF’s global network of labs.

In comparison to DNA barcoding, next-generation DNA sequencing is highly specific and can identify species in highly processed materials and complex mixtures. DNA barcoding is unable to differentiate between closely related species and is less suitable in detecting extracts as well.

Rod Wheeler, The Global Food Defense Institute

Are Food Companies Prepared for Intentional Contamination?

By Maria Fontanazza
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Rod Wheeler, The Global Food Defense Institute

Unfortunately, quite often we are reminded of the vulnerabilities throughout the food supply chain. The latest E. coli outbreak linked to Chipotle restaurants in Oregon and Washington once again has consumers and the food safety industry on edge about traceability and a company’s ability to quickly identify the source of a serious outbreak. According to the CDC’s most recent update, laboratory testing is ongoing to find the DNA fingerprint of the bacteria. Concerning as this may be, no deaths have been reported thus far, but 42 people have been reported ill and 14 have been hospitalized in Washington and Oregon. In the most recent statement released on Chipotle’s website, the company said it is “aggressively” taking steps to address the problem, including by conducting deep cleaning and sanitization of its restaurants as well as environmental testing in its restaurants, and replacing all food items in the establishments that it closed “out of an abundance of caution”.

What if this were a situation of intentional contamination? Would Chipotle or any other company in this type of scenario really be prepared? These questions were posed by Rod Wheeler, CEO of The Global Food Defense Institute during a recent conversation with Food Safety Tech about food defense, and food tampering and intentional adulteration. Wheeler and Bruce Lesniak, president of Lesniak & Associates, shared their views on the threats that the food industry is facing and why companies need to have a strong plan in place to prepare for an attack on the food supply.

During next week’s Food Safety Consortium conference, Rod Wheeler will moderate the Ask the Experts session, “Engaging Food Tampering Discussion Surrounding Food Defense” on Wednesday, November 18.  LEARN MOREFood Safety Tech: What challenges do you see companies facing in the area of food tampering and adulteration?

Rod Wheeler: Our food supply is wide open. It accounts for 13% of the overall U.S. GDP. One thing we know about terrorists is that they want to affect our financial markets. What’s the best way to do that? You attack the 13% GDP – and what infrastructure is that? It’s our wireless systems, airline systems, transportation systems, medical supply, or our food and agricultural supply. Those are the top areas in which we need to focus, and we have to make sure the food & agriculture supply remains safe and secure in the United States.

On 9/11 the world changed, and the challenge for us becomes, within all of our 18 infrastructures, but how have we changed? Do we continue to do business the same way we always have, even prior to 9/11? Over the past few years, we’ve seen a significant increase in terroristic activity around the world—from France to Syria to Yemen to Pakistan. Here in the United States, we have to be mindful of what is happening.

Rod Wheeler, The Global Food Defense Institute
Rod Wheeler, CEO of The Global Food Defense Institute

We’ve always had food safety programs: HACCP, HARPC, GFSI, SQF, etc.—those are good for unintentional contamination. But what happens if someone wants to intentionally place a deadly contaminant into a product?

In this country, on a daily basis we see contaminations occurring.  We were recently notified of a massive outbreak of E. coli that has occurred throughout the Chipotle system: 47 Chipotle stores have been closed. What does that mean? Is that just a food safety issue? What if that E. coli could have been intentionally grown in a test tube and placed into the food supply? Going forward, we have a duty and an obligation to look at these things, not just at face value but think about whether they are intentional events.  

FST: Where are the biggest holes within food defense plans?

Wheeler: With more than 15 years of visiting food processing facilities, agricultural farms, dairy farms, and dairy processing facilities, the biggest concern that resonates with me is the fact that the culture of security is not there. The culture of security is simply security awareness—not planning. People in food plants are being taught to be mindful not vigilant. The largest of food companies have well thought out and active safety and defense plans, and their employees are educated, trained and empowered. We find that this falls off sharply with the mid-sized and small manufacturers and suppliers.  All food providers must have a comprehensive and strategic security plan that is active and measureable.

For example, let’s say a contractor is walking though a food plant. You have worked in that plant for five years but have never seen this person before. Would you question that person about their credentials? Are people thinking about the things they can personally do to reduce or mitigate the risk… are they empowered?

Darin Detwiler of STOP Foodborne Ilness, PCA sentencing
“When Someone Dies, It’s Not Business as Usual”: Darin Detwiler of STOP Foodborne Illness discusses the impact of the PCA sentencing on the food industry. Watch the video

So, the question is “what do you do when/if”: This is one of the topics we will be discussing at the [Food Safety Consortium] conference. It’s interesting that when we present this scenario to the management of a food company, many answer back with a blank stare. We ask, do you shut down your facility? Do you notify your customers? Do you notify the national media? This question goes to the root of the company’s security culture and the strength of its strategic planning. Until we develop the necessary plans, processes and protocols to respond proactively, we will continue to remain vulnerable.  

FST: Do you think many food companies assume something catastrophic won’t happen to them?

Wheeler: I always ask why it is that we don’t anticipate these things in advance. People are complacent. “It’s not going to have happen here,” they say. “What terrorist would come to our small town and do this? We’re just a small mom and pop [business].”

Recently, I received a call from a 17-employee company in Tennessee. This particular company processes honey for 100 large box retail stores. I received a call from the CEO who said, “My client wants us to have one of those vulnerability things.” He was referencing the vulnerability assessment. He said, “I don’t know why they’d want us to have one of those. We’re a small company down here in Tennessee, why does my client think some terrorist would come here?” The fact is, attackers will find the weakest link to attack: The small honey company is not the target; they are the vessel by which the attackers get to the primary target, and in this case, the big box retailer. The big box retailer/supplier is the target and the simplest, most effective way to get to them is through the hundreds of small, low to no protection suppliers.

These are the issues we need to enlighten and educate companies about; we need to get them thinking differently, because this way of thinking is completely different. If you ask someone who’s been in this industry for years, they’ll say, we never had to worry about locking our doors, or use biometrics to gain access to certain areas. We never had to think about these things in the Food & Ag supply before.

During our front line training course, we place a significant amount of focus on the food plant blending areas and why it is the number one threat area for intentional/unintentional contamination of our food supply in the United States. The blending area is exposed to a number of vulnerabilities and once attacked, the tainted ingredients are spread among numerous products that once distributed, are not necessarily quickly traced once they are blended into the final product.

Bruce Lesniak: The consequences of such an emergency are multifaceted; they affect the consumer and their product confidence, the manufacturer through recall and the retailer through recall, brand damage and loss of consumer loyalty. Often, this ripple effect begins with the small supplier and works its way upstream to affect the entire process.

We are seeing this scenario unfold in real time with Chipotle—this is huge in the food industry. FDA has not been able to determine exactly where that genetic fingerprint has originated resulting in location closures, shaken consumer confidence and brand damage. –Rod Wheeler

FST: What will it take the industry to wake up to what could become a serious reality?

Wheeler: Unfortunately it’s probably going to take a major incident for people to wake up and smell the coffee. With that said, we firmly believe that it is critical to awaken the sleeping giants before something happens. We must increase the awareness and provide education to heighten the reality of what can potentially happen and promote proactive engagement of risk mitigation.

FST: In the context of FSMA, are companies prepared for the compliance stage?

Wheeler: Over the years, I’ve seen a number of companies begin to ramp up security at their facilities. But a number of them are doing it because they realize they need to comply with the food defense elements of FSMA; the larger companies are driving compliance and are requiring that their suppliers comply. But I think convincing companies about “Why” this is important, is the challenge. Often times companies will say, “we’re doing this training”, or “we’re doing this vulnerability assessment because it’s a requirement of FSMA.”

We feel that if being compliant is your “Why “reason, then you are spending time and money for the entirely wrong reason. You don’t do vulnerability assessment or training in food defense because you want to comply with the law. You do it because you want to protect your company and the consumer from the reality of what can happen and proactively work to avoid a threat.

Lesniak: We see the adoption trend take hold as it has traditionally, in three phases. First are the early adopters—they understand the importance of compliance for the right reasons and the need for food defense, Second are those who feel the urgency to comply due to a compelling issues (an incident or have been instructed to do so by larger suppliers in order to retain contracts), and third are those who will come kicking and screaming.

Wheeler: A lot of the requirements of FSMA were generated as a result of the PCA event in 2009. The prosecution and subsequent conviction of the Parnell brothers isn’t the last prosecution we’re going to see for someone violating a food safety protocol. This is the first, and it’s a wake up call.

Integrated informatics and food labs

Using Data to Ensure Food Chain Security

By Maria Fontanazza
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Integrated informatics and food labs
Integrated informatics and food labs
Integrated informatics enable labs to execute and manage all lab processes easily, with the data rigor and intelligence that lab managers require to drive efficiency and profitability, for the lab and for the business. Image courtesy of Thermo Fisher Scientific. (Click to enlarge)

Moving forward, if food manufacturers, suppliers and distributors want to be ahead of the game, they’ll need to have the ability to view their product throughout the supply chain. During a discussion with Food Safety Tech, Trish Meek, director of product strategy at Thermo Fisher Scientific, explains the importance of product traceability in the food chain, from both a consumer and food producer’s perspective.

Food Safety Tech: In your recent article about Integrated Informatics, you cite it as an ideal solution to modernizing a highly distributed food chain. What are the challenges you see companies facing in managing their global supply chain?

Trish Meek: We’ve seen the issues related to intentional adulteration documented throughout the media, and they extend to traceability. For example, what Tesco experienced during the horsemeat scandal wasn’t necessarily intentional adulteration, but rather a matter of not understanding the supply chain. Horsemeat was introduced in France as legitimate meat and then it ended up in the UK. In this case, you have a lack of traceability and thus a lack of understanding of what has happened to your product in its lifecycle.

Trish Meek, Thermo Fisher Scientific
“With consumer demand for foods that are free of gluten, GMOs and antibiotics, it’s becoming more important to customers that they understand everything that has happened to the animal and the food source.” –Trish Meek

In this complex world of suppliers, distributors and food producers, having the ability to pull in analytical data and manage it regardless of the source (whether it’s from the initial ingredient supplier or the final manufacturer) is a critical piece in understanding the overall lifecycle picture. An integrated informatics solution provides a single source of truth for that information: From the technician operating the lab process to the lab manager who is overseeing to the integration into the enterprise-level system. It provides a complete view on everything that has happened to your data, while also enabling the management of regional specifications.

FST: What are the biggest concerns in the area of food chain security?

Meek: Traceability is key, and the common denominator is food chain security: Ensuring that you’re providing security and with an understanding of everything that happened to your product, which leads to quality assurance and brand security.

FST: What are the concerns related to food chain security?

Meek: There are a few concerns:

  1. Adulteration
  2. Correct label claims. For example, 30% of the populous is trying to avoid gluten. While 1% is truly allergic to it, there’s a lot of gluten intolerance. Take, for example, recent commercials from Cheerios saying they are ensuring traceability and can say with confidence that their product no longer comes into contact with wheat in any part of the process. There’s an understanding that consumers want to believe what’s on the label, from both a health and allergy perspective as well as a concern in the public around unhealthy ingredients added or antibiotics used. As a food producer, you want to make sure you can honestly state what has happened to the food and that what you’ve put on your label is true. People are willing to pay a premium, and so there’s a drive towards the premium of being able to claim no GMOs on a label or an organic product.
  3. From a food producer’s point of view, having traceability from all suppliers is key. They want to ensure that any raw materials have been handled and managed with all the same scrutiny and adherence to regulatory requirements as their own processes. With ingredients coming from all over the world, manufacturers are relying on multi-sourcing ingredients from places they don’t necessarily control, so they need to have the traceability before the ingredients appear in the final product.

Using an Integrated Informatics Platform

Trish Meek: Through an integrated informatics platform, users can manage the entire lab process and integrate it into the enterprise system. Having the ability to incorporate the lab data is critical to ensuring product safety, quality and traceability throughout the entire supply chain. Because the solution encompasses lab processes and required lab functionalities, it enables efficiency both in the laboratory as well as across the entire operation. The solution provides an opportunity not just to the top-tier food producers but also the regionally based middle-tier companies that want to set themselves up for future growth.

The reality of the regulations today is that you must look towards the future. Twenty years ago, we weren’t including information about what nuts were present in the labeling. Now there’s consumer awareness and a change in labeling. And five years from now, there could be a different allergy that needs to be documented in the labeling. Integrated informatics gives you the business agility to take on that next step of analysis and adapt to the marketplace.

Granulated sugar with dark foreign particles

Food Investigations: Microanalytical Methods Find Foreign Matter in Granular Food Products

By Mary Stellmack
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Granulated sugar with dark foreign particles

The upcoming implementation of FSMA will likely result in increased scrutiny of contaminants in food products. If the foreign matter can be identified, steps can be taken to eliminate the source of contamination and avoid future losses of product. Small foreign particles are sometimes observed in drums of bulk granular or powdered raw materials. While these foreign particles may be seen as dark specks in the product, they are often too small for standard QA/QC methods of analysis. Microanalytical techniques, however, can be used to isolate and identify the specks. This article describes a case study of dark particles in a granulated sugar sample.

Microscope Exam

Ideally, when conducting contaminant analysis, all sample manipulations take place in a cleanroom to eliminate the chance for contamination by extraneous environmental debris. This is especially important when working with small contaminant particles, which may consist of environmental debris such as metal particles, fibers and other types of dirt. If the unknown particles are identified as common environmental debris, the analyst must be certain that he or she did not introduce any debris while handling the unknown sample.

Granulated sugar with dark foreign particles
Figure 1. Granulated sugar with dark foreign particles, 13X (Click to enlarge)

The first step in the identification process involves examination of the sample under a stereomicroscope. Figure 1 is a photomicrograph of dark brown particles, less than 1 mm in size, in the sugar sample. Particles of this size must be isolated from the bulk product prior to analysis in order to correctly identify them.

Since all of the dark particles are visually similar, only a few representative particles need to be isolated. The contaminants can be isolated by removing a small glob of tacky adhesive (50 µm or smaller) from a piece of tape with the pointed tip of a fine tungsten needle. The adhesive-coated needle tip is gently touched to the surface of one of the dark particles, causing the particle to adhere to the needle, and the particle is transferred to a glass slide or other substrate for further examination.

Isolated dark foreign particles
Figure 2. Isolated dark foreign particles, 63X. (Click to enlarge)

Figure 2 is a photomicrograph of three dark particles, isolated from the sugar granulation. The dark brown particles have a smooth, shiny appearance with conchoidal (shell-shaped) fracture surfaces, and are visually consistent with glass. However, when probed with the tungsten needle, the particles are found to be brittle and fragile, and this texture is not consistent with glass. Therefore, chemical analysis is needed to identify the brown particles.

Micro-FTIR Analysis to Identify Organic Components

Most organic compounds (and some inorganic materials) can be identified by Fourier transform infrared (FTIR) spectroscopy. For the analysis of small particles, a microscope is coupled with a standard FTIR system; this method of analysis is known as micro-FTIR analysis. The micro-FTIR system passes a beam of infrared radiation through the sample and records the different frequencies at which the sample absorbs the light, producing a unique infrared spectrum, which is a chemical fingerprint of the material. By comparing the spectrum of the sample with spectra of known compounds from a reference library through an automated computer search, the sample can often be identified.

In order for the FTIR analysis to work, the sample must be transparent, or thin enough to transmit light. In the case of the particles from this case study, this is achieved by applying pressure to a ~50 µm portion of the sample until it forms a thin transparent film. This film is placed on a salt crystal for micro-FTIR analysis.

An FTIR spectrum of crystalline sugar is shown in Figure 3, and a spectrum of a brown particle is shown in Figure 4. The spectrum of the brown particle has some similarities to sugar, but there are fewer peaks, and the remaining peaks are rounded, consistent with a loss of crystallinity. The loss of crystallinity, coupled with the brown color of the particles, suggests charred sugar.

FTIR spectrum of granulated sugar
Figure 3. FTIR spectrum of granulated sugar. (Click to enlarge)

Figure 4. FTIR spectrum of a dark foreign particle, microanalysis
Figure 4. FTIR spectrum of a dark foreign particle. (Click to enlarge)

SEM/EDS to Identify Inorganic Compounds

The FTIR method does not provide complete information about the presence or absence of inorganic materials in the contaminant. To complete the analysis of the brown particles, scanning electron microscopy (SEM) combined with an energy dispersive X-ray spectrometer (EDS) detector is needed. Using the SEM/EDS method, two types of information are obtained: SEM provides images of the sample, and the EDS identifies the elements that are present.

SEM/EDS analysis of a dark foreign particle
Figure 5. SEM/EDS analysis of a dark foreign particle

A brown particle was mounted on a beryllium stub with a small amount of adhesive, and submitted for SEM/EDS analysis. Figure 5 includes an SEM image of the particle, and a table of EDS data. The SEM image provides some information about the composition of the particle. This image was acquired using backscattered electron mode, in which heavier elements appear lighter in color. The image displays light colored specks scattered across the surface of the particle, indicating that more than one type of material is present. The light-colored circle on the SEM image shows the area that was included in the EDS analysis (the entire particle was analyzed). Looking at the column in the table for weight percent (Wt%), the particle consists primarily of carbon and oxygen, with small amounts of chlorine and iron. Carbon and oxygen are chemical constituents of sugar, but chlorine and iron are not.

SEM/EDS analysis of specks on a dark foreign particle
Figure 6. SEM/EDS analysis of specks on a dark foreign particle

The EDS system can also be used to focus on individual small areas on the particle. Figure 6 includes EDS data from five specific light-colored specks on the surface of the brown particle. The specks contain major amounts of iron with small amounts of chlorine, and sometimes chromium and silicon, plus contributions from carbon and oxygen from the surrounding sugar matrix. The composition of the specks indicates steel corrosion, likely from low alloy steel. The presence of chlorine suggests that a chlorinated substance was the initiator for the corrosion process.

In some cases, steel corrosion can be the sole cause of brown or dark discoloration of small particles. In the case of this brown particle, the SEM image shows that the iron-rich particles are not evenly distributed throughout the particle, but are only scattered on the surface. Charring is the most likely cause of the overall brown color of the particle.

Conclusion

When examined under the microscope, the dark particles in the sugar sample had the visual appearance of glass. However, chemical microanalysis of the particles revealed that they were not glass at all, highlighting the importance of microanalytical methods in determining the identity of the foreign matter. The brown particles were ultimately identified as charred sugar particles with scattered specks of steel corrosion (likely from low alloy steel) on the surface. This information can be used to narrow down the search for possible sources of the brown particles in the bulk sugar sample. As part of a root cause investigation, samples of dark particles from various locations in the manufacturing and packaging processes can be studied by the same techniques to look for a match.

More information about FTIR analysis is available in the webinar, Preparation of Polymer Samples for Microspectroscopy

Steps to Avoid a Food Crisis

By Maria Fontanazza
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Part two of Food Safety Tech’s interview with Alan Baumfalk, lead auditor and technical manager for Eurofins food safety systems, discusses how companies can reduce their chances of having a food crisis. “Sometimes we forget that part of our crisis management team is part of food defense,” says Baumfalk.

Food Safety Tech: Can you discuss the importance of the food defense plan within crisis management?

Alan Baumfalk: We need to defend the product within our facility, and we need to determine as part of the food defense plan the methods that we’re going to implement to prevent adulteration of product.

We need to step up and watch this: The process literally travels from farm to fork; from the crop through processing through distribution and to the final consumer. As part of our food defense plan we need to protect sensitive processing points from intentional adulteration, and we must watch for potential accidental adulteration.

It is important to carefully control the activities in the plant. Part of that involves limiting employee, subcontractor and visitor access to production equipment, manufacturing, and storage areas by designating access points.

These steps can help to eliminate issues involved in causing a crisis:

  • Secure the storage of raw materials, packaging equipment and hazardous chemicals
  •  Control all chemicals within the facility, because they can be used to deliberately or accidentally contaminate food.
  •  Hold finished products in secure storage.
  •  Control transportation. Apply seals to the full truckload.
  •  Monitor all points of distribution.