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.
Across the board, increased employee awareness and training has become a big issue in food safety. The foodborne illness outbreaks that hit Chipotle Mexican Grill has put retail and restaurant establishments on high alert, yet this is just another example of the reactive culture in which we operate, according to Matt Schiering, vice president and general manager at Sani Professional.
“Think about your own restaurant experiences. Guests don’t want to see or be confronted with a greyish brown rag [that is used to] wipe a table, then wipe a seat, then wipe an adjacent table. It just screams unclean,” says Matt Schiering of Sani Professional.Food Safety Tech recently hit the road with Schiering and John Caton, regional sales manager at Sani Professional, to experience first hand how one company is communicating its message to customers. Breaking with tradition has been an important part of promoting cleaner technology: The use of the rag and bucket as a means to clean both the front of the house (tables, chairs, counters, etc.) as well as the back of restaurants and retail establishments, while still fairly common, has outlived its effectiveness, and frankly, says Schiering, “screams unclean”. Caton and Schiering continued the conversation with their customers about how using disposable wipes for cleaning, sanitizing and disinfection helps prevent the spread of contamination, along with the cost savings associated with using such products. The company takes a multi-prong approach to promoting awareness among its current and potential clients, from deploying a sales force that directly interacts with quality assurance and food safety professionals in establishments to offering how advances in sustainable technology can help them stay ahead of the curve to driving consumer advocacy.
Food Safety Tech: How is Sani Professional raising the level awareness of the disadvantages of the traditional cleaning method (the rag and bucket method) in the retail environment?
Matt Schiering: There are a few ways to raise the level of awareness. The first and foremost is “feet on the street”. We’ve deliberately moved toward a direct-to-customer sales force, which gives us the opportunity to interface directly with QA, food safety and operations to show them a simpler, more efficient, more effective, and guest appealing way versus the traditional rag and bucket. The first win is one for the user (the employees of a given establishment), because associates have shown us time and time again that they do not like the mixing and measuring, and the errors that are often associated with that process. They don’t like the dirty rag itself—having to fish it out of the bowl and then present it or be seen with it in the front of the establishment. It’s a win for the operator (the manager), because with our system, there’s no longer any heightened heart rate when the health inspector shows up. One of the most common violations is the water in the buckets being out of spec or the rags themselves not being inside the bucket per regulation. And perhaps most importantly, it’s a win for the guest. Think about your own restaurant experiences. Guests don’t want to see or be confronted with a greyish brown rag [that is used to] wipe a table, then wipe a seat, then wipe an adjacent table. It just screams unclean.
As we talk about the evolution in perception, away from traditional methods, we believe that speaking directly to the consumer has to play a role. There has to be a degree of consumer-driven advocacy for a better way. – Matt Schiering
FST: Regarding employee training, how should retailers be more proactive in ensuring their employees are engaging in proper food safety practices and aren’t spreading foodborne illnesses?
Schiering: It varies by chain. Unfortunately, we live in a reactive culture—and that goes well beyond the restaurant industry.
Oftentimes a problem precedes a protocol or other means of addressing said problem. Chipotle is one example: They’ve taken an exhaustive look at restructuring their food safety protocols as a result of a myriad of foodborne illness-related issues that they suffered in the preceding months. The [retailers] who are doing it best are the ones who build it into their establishment in the first place where it’s not predicated by some sort of problem. That involves training materials, in-service lessons, and online training (i.e., ServSafe certifications). Waffle House, for example, has Waffle House University where food safety is a key component to that system.
We envision ourselves as part of that process. We take a microcosm—the notion of proper food handling, prevention of cross contamination related foodborne illness—and provide an innovative and easy-to-use solution, and all the training and collateral materials associated with the solution that explain the proper use. We also provide test kits so that if the health inspector wants an in-the-moment proof that our product is doing what the label says it does, [the retailer] can provide that at a moments notice. It becomes more of a service proposition than simply a product-driven solution.
Using disposable wipes for cleaning, sanitizing and disinfection can help prevent the spread of cross contamination and foodborne illness.
FST: Where do you see sustainable products fitting into the space?
Schiering: This also boils down to education, because the perception of disposables is that they’re wasteful, when in fact they needn’t be any more costly than existing solutions.
If you’re using a linen service, there’s a cost associated with renting towels, but there’s a higher cost associated with wasting towels. So if a towel ends up in a gym bag or in the trash because of overuse and/or abuse, there’s a significant upcharge for not returning that towel to the rental agency. That’s what we call the hidden cost or the dirty little secret of rag and bucket sanitizing. When you factor that in, and everyone [retailers] experiences that type of loss, and you look at the fact that sanitizing wipes kill pathogens trapped in the wipe as well as whatever it is coming into contact with at the surface, thereby enabling it to be used on multiple surfaces without causing cross contamination—the cost aligns very closely. And of course it’s a more value-added guest experience than a dirty rag being used from table to table, which is not preventing cross contamination.
Speaking to the environmental piece: At the moment, we’re actually fairly well ahead of the industry. It varies chain to chain—some chains are doing a better job than others, because it’s part of their corporate culture. But by providing solutions that are leveraging either recyclable substrates or compostable substrates, we provide greater opportunity to reduce the environmental impact often associated with disposable products. If a retailer is working with a waste management partner that can handle industrial compostable products or non-solid state recyclables, we have solutions that are appropriate for those operations, so that we’re not just adding to landfills but rather essentially recycling and/or regenerating the products that are being used, and at no greater cost.
Most retailers haven’t gotten there yet. It speaks directly to corporate culture and corporate mission of the end user. We deliberately target customers who are a little bit ahead of the curve when it comes to “green technology or “green behavior”. And so when the rest of the industry catches up, we’re more than ready to serve them with products that meet those needs.
FST: Where do consumers fit into the picture, especially has industry moves away from traditional methods in food safety?
Schiering: About a decade ago, consumers started demanding that retailers like Walmart, Target, and local grocers provide a means of sanitizing shopping carts when they walk into their local retail establishments. There were myriad news reports about the germs and potential for contamination and illness arising from the often used and rarely cleaned implements—these vehicles for placing your groceries. We answered the call a decade ago, and at one time it was a significant piece of our business. It continues to be a marketplace we serve, albeit a much commoditized one. But the rise in that solution would not have taken place if not for consumers advocating for a better way.
We’re starting to create a presence on Facebook and other social media outlets to remind consumers that it’s up to them in many cases to ask for, if not demand a more effective, more pleasing way of ensuring their safety in dining establishments. Unfortunately, incidents like what we saw at the large Mexican food service retailer do ultimately play a part in that consumer advocacy, albeit a negative one, because we are a reactive society. But by presenting a positive message and sharing alternatives in the absence of citing examples or shaming retailers through the problem, we believe that will be one of the keys to changing perceptions at the retail level.
Implementation of FSMA will result in greater scrutiny of foreign material in food products at every stage of production, as well an entirely new pressure to locate and eliminate the source of contamination from the supply and production chain. Identifying foreign materials found in food products is the first step in determining their source, and therefore in determining how to prevent a given foreign material from being introduced into the product. For identification of small particles ranging from 1–1000 µm, microanalytical techniques are essential.
Examining and Isolating Foreign Material
Before the foreign material is prepared for analysis, the material is examined under a stereomicroscope. Ideally, isolation of the foreign particles from the host matrix and preparation of the foreign particles for microanalysis is performed in a cleanroom, which mitigates the introduction of environmental contamination not related to the initial contamination problem.
Figure 1. Particles filtered from a liquid product.
Under the stereoscope, the foreign material is isolated from the product matrix using a tungsten needle probe. It is photographed and the physical characteristics of the material (color, elasticity, magnetic properties, etc.) are observed and documented. Figure 1 shows particles filtered from a liquid product. In this case, the particles are approximately 100 μm and smaller. Most of the particles appear black to dark brown/orange in color. Some are brittle, while others are not. All are magnet responsive.
Only a few particles must be picked and prepared for analysis in this case because the particles are roughly similar. The coloration of the particles, along with their mechanical properties (magnetic, brittle, hard) indicate that the material is likely inorganic; scanning electron microscopy with energy dispersive X-ray microspectrometry (SEM-EDS) could be used to determine the elemental makeup of the material. The coloration and mechanical properties imply the source of the particles could be production machinery.
Figure 2 (click to enlarge)
Identifying Inorganic Compounds with SEM-EDS
In a scanning electron microscope, a beam of electrons is scanned over the particle producing several signals, some of which are used for imaging, and some that are used for elemental analysis. For this discussion, the signals of interest for elemental analysis are X-rays. The energies of the X-rays are characteristic of the elements found in the sample. By counting these X-rays and arranging them according to their energies, a spectrum is produced, and elements in the sample can be identified and quantified.
Figure 3 (click to enlarge)
Figures 2 and 3 are SEM-EDS data from one of the brittle particles from the filter. The particle is steel corrosion (iron, chromium, and nickel), possibly with brass corrosion (copper and zinc) and some silicate material (elevated silicon and aluminum). Residues of corrosive agents (chlorine and sulfur) are present. The inclusions analyzed are 300 series stainless steel (see Figure 2). SEM-EDS data from one of the harder dark particles is shown in Figure 4. This particle is oxidized 300 series stainless steel, likely Type 316. 300 series stainless steels are not generally magnetic, but magnetism can be induced during wear processes.
Figure 4. SEM-EDS data from harder dark particles. (click to enlarge)
Stainless steels, particularly Type 304 and Type 316 are common in food manufacturing environments. Pinpointing the source of these materials as contaminants can be frustrating due to the number of pieces of equipment made from these alloys. However, other metals are less common, such as Waukesha 88, a bismuth containing nickel-based alloy that is used in pump rotors and other moving parts because of its wear properties. Another less-common alloy is Type 321 stainless steel, a titanium stabilized stainless steel that is used in high temperature equipment where corrosion resistance is needed. Materials such as these are more easily traceable to their source, and therefore more easily repaired and thus eliminated as a source of foreign particles.
Figure 5. Glass particle. (click to enlarge)
Other inorganic materials, such as glass, are also amenable to identification by SEM/EDS. SEM-EDS data from a glass particle is shown in Figure 5. Often, the glass can be identified as soda-lime glass or borosilicate glass. Soda-lime glass is commonly used for glass containers and bakeware; it is a mixture of oxides, mostly silicon dioxide, sodium oxide, and calcium oxide with smaller amounts of other oxide compounds. Borosilicate glass, commonly used in heat-resistant labware, contains silicon dioxide with a few weight percent boron trioxide, along with other oxide compounds; its composition results in a low coefficient of thermal expansion, and it is used in applications where its chemical and heat resistance are necessary. Identifying the glass type is helpful in determining the source of glass particles.
Figure 6. Reference spectrum for Viton. (click to enlarge)
The SEM-EDS method cannot uniquely identify organic compounds, as it provides only elemental information—an EDS spectrum of organic material shows major carbon, and if it is degraded, oxygen. Protein will contain nitrogen as well.
Figure 7. Cellulose IR spectrum. (click to enlarge)
FTIR analysis can identify most organic and a few inorganic materials. For small particles, micro-FTIR (an FTIR system with a microscope coupled to it) is used. Micro-FTIR analysis requires that the sample be thin enough to transmit light, since the system passes a beam of infrared radiation through the sample and records the frequencies at which the sample absorbs infrared radiation. The spectrum from a given material is unique, and even mixtures of materials can often be identified by comparison to known spectra from a reference library using an automated computer search.
Figure 8. Cardboard IR spectrum. (click to enlarge)
In this way, organic materials such as Viton O-rings can be identified (Figure 6 is a reference spectrum for Viton). Other organic material may be present in the product, such as cellulose (see Figure 7) or cardboard (see Figure 8). While these materials are not dangerous as small particles, they are not desirable in food products. When these kinds of things are found, tracing them to their source may be simple (as in the case of the O-ring material) or hard (cellulose can come from paper or cotton clothing, for example).
If the organic material found has inorganic fillers like titanium dioxide or silicon dioxide, then SEM-EDS can be used in concert with the micro-FTIR to refine the material description and simplify the process of identifying the source of the foreign material.
When used in tandem, SEM-EDS to identify inorganic materials and micro-FTIR to identify organic materials can be powerful tools for determining the origin of foreign particles. These microanalysis methods are essential tools for identifying and tracing the source of contaminant particles in food.
While the United States has no legal definition of food fraud, current thinking tends to be focused primarily on companies and products involved in the illegal substitution of one ingredient for another in a product. Such substitution generally involves substituting a cheap filler in the place of the labeled ingredient. In recent news, Parmesan and Romano cheeses have captured news headlines because of illegal “misbranding” of foods meaning that the label on shredded cheeses from companies like the Castle Cheese, Inc. company in Slippery Rock, PA include ingredients found through FDA testing that are included in percentages beyond allowable levels. In the case of shredded cheeses, so called “imitation” cheese better is known as wood pulp. The labels stated that the ingredients were 100% cheese.
Perhaps Slippery Rock is an apt name for the Castle Cheese operation where the inclusion of wood pulp was cheaper than the inclusion of real parmesan cheese. Such activities are becoming increasingly known as “economically motivated” and the practice is one of economically motivated adulteration. The FSMA final rule, Focused Mitigation Strategies to Protect Food Against Intentional Adulteration, will make these practices illegal.
Such intentional cheating has a long record in the history of food. No one really knows the extent of such food fraud activities, when they started (perhaps at the beginning of time?), or who could claim to be the first person to win an international award for creativity.
There are so many ways to commit food fraud that it boggles the mind and creates an almost complete inability on the part of governments, testing laboratories, food processors, retailers and the public to identify, let alone fully prevent and capture the guilty every single time.
Think about a few things. Is it fraudulent to leave the identification of GMO ingredients off of labels? If a packer knowingly packs a product in dirty packaging, is that practice fraudulent? If the food safety part of the government knows how high the levels of fecal coliform are on most of the produce we eat but does not acknowledge the problems or inform the public, is this practice fraudulent? How about the idea that a retail outlet replaces an “expired” label on hamburger with a new unexpired label? Or how about the time Sysco was shipping perishable foods in refrigerated trucks and storing eggs, milk, meat, chicken and other products in the same storage sheds where you might keep leftover junk from your garage? Do “Good Things Come From Sysco”?
But none of those examples have anything to do with intentionally substituting a cheaper ingredient for an ingredient on the label. Honey, olive oil, coffee, juices, fish, alcohol, milk and dairy products, fish, vitamins, meat, spices, organic foods, maple syrup, peanut product, flavorings, preserves, cereals, colorings, wines, vinegar, purees, sweeteners ,and other ingredients are involved. And food fraud occurs in manufacturing, processing, packing and food holding operations. Such large opportunities for all foods in all operations means the entire food chain is—at one time or another, in one place or another—suspect.
The Grocery Manufacturers Association (GMA) estimates that food fraud may cost the global food industry between $10 billion and $15 billion annually with lost sales between 2% and 15%. They estimate that approximately 10% of all commercial food products are impacted.
Considering the fact that the food industry claims their profit margins are only a few percent, it would seem that if they wanted to reduce food costs, food fraud would surely be a prime business improvement target. And GMA, unfortunately, is also focused on economically motivated adulteration such as unapproved additives, mislabeling, counterfeit ingredients, transshipment (shipping from one country to another to repackage and relabel in order to avoid taxes), and dilution.
When a consumer enters a supermarket in search of fresh meat, poultry or fish to cook for dinner, he or she knows little about how those products were packaged. Adding water to the pad that is often inserted under the meat to soak up blood, adds weight to the scale and money to the price. Packing the meat using carbon monoxide is common in order to “preserve” the product color. Red meat should look red, right? While the FDA considers this practice generally recognized as safe (GRAS), studies regarding how carbon monoxide interacts with the foam packaging and the clear plastic wrap covering the package are nonexistent. What makes the practice deceptive is the lack of information on the label that tells consumers carbon monoxide is used to preserve color. Of equal importance are recent studies that clearly show that many of the plastics used in today’s food packaging operations contain toxic chemicals shown to be dangerous to humans.
‘Food fraud is a collective term used to encompass the deliberate and intentional substitution, addition, tampering, or misrepresentation of food, food ingredients, or food packaging; or false or misleading statements made about a product for economic gain’.
After the monster European horsemeat scandal (remember that one?) in which horse meat was substituted for beef to the embarrassment of many companies, such as Burger King and Ikea, the United Kingdom promised proactive solutions from food laboratories and improving supply chain audits in an effort to slow and diminish the number of incidents reported annually.
In the United States, we frequently point to the melamine (milk substitution) in baby formula or the pet food problems that came out of China as evidence that foreign companies are primarily to blame for food fraud. Coupled with governmental trade agreements and the attitude that other countries are dumping substandard product on American consumers, it seems easy to blame others for food fraud –except for the fact that we in America are dealing with so many incidents.
The problem with our inability to tackle food fraud in part comes from the gap between our ability to identify and develop appropriate and targeted food ingredient testing capabilities. So many types of food, so many types of tests, so many types of ingredients, and so many types of ways to intentionally or accidentally cheat the system all combine to confuse and confound our efforts to quickly and economically establish detection systems.
In most food distribution arenas, food traceability systems are slowly being agreed upon and implemented. However, the FDA does not seem to be able to help with establishing data and other standards that would help establish traceability requirements designed to quickly and accurately get to the source suppliers in food fraud events. Other industries under FDA medical device and drug laws have worked to establish solid chain of custody systems. Chain of custody implies that the suppliers and handlers are legally responsible and clearly identified. Leadership in this area is clearly needed.
While there are many good resources evolving both within and outside of the United States, those resources are scarce and relatively immature. It seems that without some basics, such as legal definitions, standardized testing practices, and an agreement that food fraud is much more than substitution of one ingredient for another, we have a very long way to go if we expect to get the food fraud system under control.
Monitoring for veterinary drug residues is conducted to ensure food safety and compliance with approved veterinary medicine practices. Veterinary drugs are used in animal husbandry for a variety of reasons, including as a curative/preventive of disease in herd and flock, to improve meat quality, and to promote growth. The chemical classes of drugs that may be used are broad, but major classes include antibiotics, anti-parasitics, and hormones. While risk-modifiers are used to minimize risk for consumption, residues from these drugs, their breakdown metabolites, or associated impurities of the drug may persist in animal tissue, necessitating the requirement that contaminant testing be undertaken.
In the United States, trace analysis of contaminants in food products began in the early 1970s following amendments to the Federal Food, Drug, and Cosmetic Act (FFDCA) in 1968. Worldwide, the regulatory requirements for contaminants in food have seen significant tightening due to a number of high-profile contamination crises and increased trade of food across country borders. From the technology standpoint, lower detection limits have been made possible by improvement of the detection capabilities of the analytical methods and instruments. Some of the most stringent requirements for contaminants in food are found in the European Union, where the levels of contamination should be below Minimum Residue Limits (MRLs), whereas in the United States, such limits are called U.S. tolerances.
Image courtesy of MilliporeSigma
When analyzing for drug residues, the choice of tissue has historically been the liver and kidney tissues, as these organs serve to remove the contaminants from the body and, as a result, the concentration of contaminants there is higher and easier to detect. Muscle tissue now often is added to the target list, as its contamination would have a direct impact on consumers.
With regards to veterinary drugs testing, one can distinguish between screening methods and confirmatory methods. The former should be fast and high-throughput and used to detect the presence of an analyte. The confirmatory methods should be able to provide confirmation of an analyte’s identity and quantitation at the levels of interest. Microbiological methods were popular for screening of antimicrobial drugs since these drugs inhibit growth of microorganisms, but suffer from a lack of specificity since not all microorganisms are equally sensitive to all antibiotics. Rapid screening methods include immunoassay-based testing kits, which are specific, fast, and can include multiple antibiotic classes in one test. Confirmatory methods typically include chemical analysis techniques with LC-MS detection, which provides the best ionization for most classes of veterinary drugs, along with better selectivity for focused analysis and lower detection limits. LC-MS can provide specific analysis of compounds from multiple classes in the same run through either targeted MS/MS or non-targeted analysis of unknowns through high mass resolution methods. The speed of LC-MS analysis has improved with the introduction of ultra-high pressure liquid chromatography-MS (UHPLC-MS) instruments. In the last few years, UHPLC-MS methods simultaneously serve as screening and confirmation methods for multiple classes, so called “multi-residue methods”. Some of these methods use MS/MS detectors and some use high-resolution mass spectrometers utilizing time-of-flight and ion trap detectors. These methods now can provide fast turn-around time and better accuracy in comparison to microbiological methods. They may be preferentially used by testing laboratories that are equipped and capable of utilizing the latest MS instrument technologies.
The 4th Annual Food Labs conference provides practical solutions and best practices on running, managing and equipping a food lab. | March 7–8, 2016, Atlanta, GA | LEARN MOREAll mass spectrometry methods that strive to perform simultaneous analysis of multiple veterinary drug classes are prone to the same drawbacks. Due to the differences in the analytes’ polarity, acidity and hydrophobicity, the quantitative extraction of analytes from tissue samples could be difficult. Ideally, the sample preparation methods should be compatible for compounds with varying physico-chemical properties but still provide selective separation from the matrix components to avoid occurrence of matrix effects during quantitation. The co-extracted matrix impurities are undesirable since they can affect the ionization of targeted analytes and result in under- or over-estimation of their concentration (ion suppression or enhancement). Due to the difficulty in designing a method that works for a wide variety of analytes, cleanup is often omitted for multi-class multi-analytes methods, and the stable isotope internal standards are used to correct for ionization effects during quantitation. However, omitting the sample cleanup could lead to other methodology problems.
As noted in the veterinary drug analysis session during the 2015 AOAC Annual meeting, sample cleanliness can result not only in matrix effects and impact quantitation, but it can also have an effect on the mass accuracy when high-resolution mass spectrometry is used and, therefore, can affect the identification of the analytes and lead to false negatives.
The most often used methodologies for sample cleanup during analysis of veterinary drugs in tissues is solid-phase extraction (SPE), both in cartridge and dispersive formats. C18 SPE proved to be a very versatile sorbent that often resulted in the best cleanup and best precision of analysis, closely followed by polymeric sorbents when applied to multi-class LC-MS analysis.
Aminoglycosides Antibiotics
Aminoglycosides is one class of veterinary antibiotics that is hard to include into multi-class methods. The aminoglycoside structures include connected modified sugars with different number of substituents including hydroxy- and amino-groups. The higher degree of polarity for aminoglycosides contributes to their solubility properties: these compounds are freely soluble in water and to some extent are soluble in lower alcohols, but are not soluble in common organic solvents and have solubility issues in solvent-water mixtures with high organic contents. Therefore, the normal extraction conditions that include organic solvents and are frequently applied to most other classes of veterinary drugs do not work well for aminoglycosides. A separate method is often used to extract and analyze these antibiotics.
Most often aminoglycosides are detected by mass spectrometry through the formation of positive ions during electrospray ionization. The LC separation of aminoglycosides could be done by either a reversed-phase (RP) method with ion-pair mobile phase additive to insure the retention of compounds or by HILIC chromatography. We have investigated both methods and looked at the sensitivity for detection of these compounds. The use of ion-pair is most often presented as a disadvantage, as it can reduce the analyte signal through the decrease of ionization efficiency and fouling the LC-MS instrument. While the use of ion-pair in our study decreased the ionization for some of the lighter compounds in this class (streptomycin, puromycin), ionization efficiency increased for the heavier mass compounds (gentamycin, neomycin). RP chromatography resulted in improved separation of the analytes compared to HILIC. LC-MS fouling from the use of HFBA was not observed in our investigation that spanned the course of a couple of years. In the HILIC mode with use of formic acid as a mobile phase additive, the detection of neomycin was problematic due to very low sensitivity. It was as low as one seventh of the sensitivity obtained by RP method.
The instrument response for aminoglycosides also depends on sample extraction and cleanup and the accompanying matrix ionization effects. The extraction from animal tissues has been traditionally done using the McIlvaine buffer that includes 2% Tricloroacetic acid (TCA) to precipitate proteins and release any bound analytes and 0.4 mM EDTA to prevent the binding of the analytes to cations and/or glass. Then the extract undergoes cleanup steps using SPE. The SPE sorbent most often used is a cation exchange phase, as the aminoglycosides have ionizable amino-groups and can be retained from the extract through ion-exchange interactions. Another option for the SPE cleanup became recently available—molecularly imprinted polymeric (MIP) SPE. MIPs, which are sometimes called “chemical antibodies”, mimic the performance of immunoaffinity sorbents. MIPs have binding sites that conform to the shape and functionality of a specific compound or a compound class. Strong binding of the analyte to the MIP makes it possible to perform intensive SPE washes that lead to very clean samples. Unlike immunoaffinity sorbents, MIPs are compatible with organic solvents and strong acids and bases.
We have tested the MIP SPE versus the traditional weak cation exchange (WCX) SPE cleanup for aminoglycosides spiked into pork tissue. The resulting ionization effects were compared as an indication of samples cleanliness. The quantitation in both cases was done using matrix-matched calibration curves and in both cases the recoveries for most of the ten tested aminoglycosides were above 70% (with exception of spectinomycin at 33% in case of WCX cleanup and tobramycin at 55% in case of MIP cleanup). For the two cleanup methods, there was a significant difference in matrix effects. In Figure 1, matrix factors close to 1.0 indicate little to no matrix influence for analyte detection: the ionization of the analyte in mass spectrometer is not influenced by co-extracted matrix impurities and quantitation values are not skewed. Values for matrix factors that are significantly greater than 1.0 suggest matrix enhancement for the analyte and values less than 1.0 are considered to be the result of matrix suppression. Significant matrix suppression was observed for all analytes when WCX SPE was used for cleanup. The ion suppression effect was significantly less for samples cleaned using MIP SPE. In addition, we observed significant time savings when using the MIP SPE cleanup method, as it did not require sample evaporation after using water-containing elution solvent.
Figure 1. Matrix factors close to 1.0 indicate little to no matrix influence for analyte detection
Conclusions
While improvement in the laboratory instrumentation allows the simultaneous and fast analysis of multiple contaminants, sample preparation remains important for reliable identification of contaminants in screening methods and error-free quantitation in confirmatory methods. Both the extraction and sample cleanup methods can contribute to accurate multi-class methods analyzing wide variety of veterinary drugs. New and upcoming technologies such as molecularly-imprinted polymers could be used for more targeted analysis of specific classes of analytes via instrumental methods.
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, 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.
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.
While illnesses linked to Chipotle restaurants are grabbing headlines, the federal government recently took steps to improve how manufacturers and packagers process and handle food. Last year FDA released several final FSMA rules, giving food companies a roadmap for ensuring food safety. The proactive approach of the regulations can help companies avoid the hazards that lead to disease and allergen contaminations, and even legal troubles. Indeed, unsafe food handling can carry costly consequences from both a financial standpoint as well as in lives lost or harmed.
In 2011, the good intentions of a family-owned cantaloupe company produced tragic results. The company, seeking more natural melons, followed a consultant’s advice and discontinued the chlorine rinse used to wash off contaminants. A Listeria outbreak followed, killing 33 people and hospitalizing 147 more. Although prosecution is rare in foodborne disease outbreaks, the company owners were sentenced to probation, home detention, community service, and $150,000 each in restitution.
A more egregious case occurred in September 2015, when the former CEO of the Peanut Corporation of America was convicted of knowingly shipping Salmonella-tainted peanut butter, which had caused an outbreak that killed nine people and sickened hundreds more. Stewart Parnell was sentenced to 28 years in federal prison.
The new regulations require companies to undertake hazard analyses of their production, along with remedial steps. This scrutiny leads to the creation of a written plan that details the controls to prevent contamination and establish a schedule for periodic testing. This analysis and control system is called the Hazard Analysis Critical Control Point, or HACCP.
Adherence to regulations doesn’t necessarily protect a company from liability, but not adhering can sound a company’s death knell when there’s a problem. The following are five ways in which companies can protect themselves:
Put food safety first. The company culture must revolve around it. The message that the HACCP plan is to be followed must be relayed to all levels of the organization. Otherwise, companies can face severe consequences, based on the question, “Did the company behave badly enough to face strong punitive damages?”
Concentrate on internal communications. In many cases, food recalls happen because of a breakdown in the communication process.
Hire accredited consultants. Make sure that your consultants are qualified and have been accredited by an appropriate body such as the International HACCP Alliance or The Seafood HACCP Alliance.
Don’t overlook supplied products. Suppliers should adhere to strict contamination-prevention protocols, but don’t assume they follow guidelines completely or have flawless processes. Your contracts with them should require that they periodically audit their facilities and share the audit results with you.
Label clearly. Packaging language might state that a product is manufactured in facilities that also process allergens such as peanuts and tree nuts. These types of warnings allow consumers to make up their own minds. It is also a reminder that HACCP plans must address prevention of cross-contamination (i.e., putting cleaning protocols in place if products with and without allergens are processed on the same equipment).
Many problems involve internal slip-ups or problems with supplied ingredients that allow contaminated food to reach consumers. If the contamination becomes known—and it often is not, when victims don’t equate their illnesses with tainted food—the businesses involved often face strict liability, meaning they carry some blame even if they didn’t act in a negligent manner and cause the problem directly.
Keep in mind that liability isn’t the only consequence of non-compliance. A recall or outbreak can damage the reputation of the company and the product. The cantaloupe tragedy sent sales of the melons plummeting, even in states not linked to the outbreak.
To minimize the hit on sales, a recall team should be in place, with a plan modeled on crisis management principles. Team members should come from all divisions of the company, including transportation and distribution to track down products, and communications to manage messaging. Legal counsel should be on board to advise on the ramifications.
When it comes to foodborne outbreaks, it’s a matter of taking classic prevention and preparation steps. Do everything you can to keep it from happening, but be ready just in case it does.
After uncovering foreign material in an incoming ingredient during the production process, Huisken Meat Company has recalled 89,568 pounds of beef patties. According to the USDA, the recall is due to concern that the products may be contaminated with “extraneous wood materials”. The Sam’s Choice Black Angus Vidalia Onion patties come in 2-lb boxes and were shipped to retailers across the country, including Walmart.
There have been no reports of adverse reactions, and the USDA is advising that consumers throw out the items or return them to the retailer.
Several news outlets have reported that the U.S. Department of Justice (DOJ) is investigating Blue Bell Creameries following the Listeria outbreak that resulted in three deaths in Kansas and 10 illnesses in Arizona, Kansas, Oklahoma and Texas between January 2010 and January 2015.
According to The Wall Street Journal, the DOJ is mainly interested in the involvement of company executives—did they know about the Listeria contamination? If so, what did they do about it?
Last April Blue Bell recalled all of its products over concerns of Listeria contamination and shut down the production line where the products were manufactured.
Blue Bell started a limited-release of its ice cream products last August. The company has not yet issued a response to the reports about the DOJ investigation, but last week it announced that it would begin a “bonus phase” of product re-entry in El Paso, Texas, Little Rock, Arkansas, and Memphis, Tennessee. This is scheduled to be followed by phase five of market re-entry in parts of Tennessee, Alabama, Georgia, Kentucky, North Carolina, South Carolina, and Virginia the week of January 18, and then shipment into all of Florida, southern Georgia and southern South Carolina the week of January 25.
The company stated in a press release that after phase five is completed, all of Blue Bell’s furloughed employees will have returned to work.
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