Tag Archives: Focus Article

Honey, adulteration

The Honey Trap: Analytical Technology Makes Food Fraud Easier to Catch

By Christopher Brodie
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Honey, adulteration

Because of its high nutritional value and distinctive flavor, natural honey is a premium product with a price tag significantly higher than that of other sweeteners. As a result, honey is often the target of adulteration using low-cost invert sugar syrups. This article looks at two analytical approaches based on isotope fingerprint analysis using isotope ratio mass spectrometry (IRMS) that can be used to detect honey adulteration and safeguard product integrity.

Honey is a complex mixture of sugars, proteins and other compounds, produced in nature by honeybees from flower nectar or honeydew. The extent to which its sugars are present is heavily dependent on the floral source and differs significantly between honeys produced in different regions. Climate, processing and storage conditions can also have an effect on the amounts of these sugars.1

Fructose and glucose are the major components of honey, and account for 85–95% of the total sugars present. The remaining carbohydrates are a mixture of disaccharides, trisaccharides, and larger oligosaccharides, which give individual honeys their own characteristic taste.

These distinctive flavors, combined with honey’s renowned nutritional benefits and a growing consumer demand for natural, healthy ingredients, have contributed to a substantial increase in honey sales over the past few decades. However, this demand has also helped to raise costs, with some varieties, such as Manuka honey, reportedly selling for as much as $35 for a 250 gm jar.

Just like many other food products that have a premium price tag, intentional adulteration is a significant concern for the honey industry. The fraudulent addition of cheaper sweeteners, such as sugar derived from cane, corn and beet sources, to extend product sales, is unfortunately common within the marketplace.

Honey producers and suppliers therefore require reliable and accurate analytical techniques to profile the composition of honey to identify cases of adulteration. Using analytical data, honey adulteration and counterfeiting can be routinely identified and product integrity can be maintained.

Carbon Isotope Fingerprints of Honey

Analysis of honey is commonly undertaken using isotope ratio mass spectrometry (IRMS) for the detection of adulteration. Honey has a fingerprint, a unique chemical signature that allows it to be identified. To visualize this fingerprint, IRMS can be used to identify the botanical origin of its constituent sugars.

Two ways that carbon can be incorporated into plants by photosynthetic CO2 fixation are the Calvin cycle (also known as the C3 cycle) and Hatch-Slack cycle (the C4 cycle). The nectar used by bees to produce honey comes from plants that produce sugars via the C3 pathway, while the sugars derived from sugar cane and corn are produced by the C4 pathway.

Carbon naturally exists as two stable isotopes that behave in the same way, but possess different atomic mass numbers. Carbon-12 is the most abundant in nature (98.9%), whereas carbon-13 is far less common (1.1%). By measuring the ratio of carbon-13 to carbon-12 (13C/12C) using IRMS, the carbon isotope fingerprint of the honey can be determined. As more carbon-13 is incorporated in sugars produced by the C4 pathway, the adulteration of honey with sugar cane and fructose corn syrups, rich in C4 sugars, can be detected.

In unadulterated honey, the carbon isotope fingerprint will be similar to that of the natural protein precipitated from the honey. However, if cane sugar or high fructose corn syrup has been added, the isotope fingerprint of honey and protein will be significantly different.

Detection of Adulteration by EA-IRMS

One approach that has traditionally been used for the detection of honey adulteration is elemental analysis interfaced with IRMS (EA-IRMS).2 This highly robust, rapid and cost-effective technique is able to reliably detect the addition of C4 sugars in honey at levels down to 7%.3 The analytical approach complies with the official method for the analysis of C4 sugars in honey, AOAC method 998.12.4

In EA-IRMS, bulk honey is combusted in the presence of pure oxygen to form CO2 for analysis. The CO2 produced from the combustion of the bulk honey, including all sugars and the protein fraction, is analyzed by IRMS. Figure 1 shows carbon isotope fingerprints of four unique samples, including bulk honey and the proteins extracted from those honeys, determined using an EA-IRMS system. In each case of adulteration, shown in the grey columns, the honey δ13C value becomes more positive relative to the protein value, moving towards the carbon isotope fingerprint of C4 plants. The natural variation of δ13C in honey is shown by the red lines.5

Figure 1. Carbon isotope fingerprints of bulk honey and protein fractions from those honeys. The red lines show the natural variation of δ13C in honey.2

Detection of Adulteration by LC-IRMS

While EA-IRMS can be used to identify cases of honey adulteration using the bulk sample, the analysis of low levels of added C4 sugars and C3 sugars (i.e., beet sugars) to honey reveal that a compound specific technique with more powerful separation capabilities is needed. Furthermore, as fraudsters develop more sophisticated adulteration techniques and effective ways of concealing their actions, it can be necessary to utilize other IRMS techniques.

Much lower limits of adulteration detection can be obtained from liquid chromatography interfaced with IRMS (LC-IRMS). This technique permits the analysis of very small sample amounts without the need for extensive preparation or derivatization, and can also identify C3 sugar adulteration, which EA-IRMS cannot readily achieve, and therefore serves as a strong, complimentary isotope fingerprint technique. There are IRMS portfolios available that allow for sequential automated analysis of both analytical techniques.

Using LC-IRMS, the sample is oxidized within the aqueous solvent eluting from the HPLC column. The oxidation reagent consists of two solutions: The oxidizing agent itself and phosphoric acid. Both are pumped separately and added to the mobile phase. Within this mixture, all individual organic compounds eluting from the HPLC column are oxidized quantitatively into CO2 upon passing through a heated reactor. In a downstream separation unit, the generated CO2 is then separated from the liquid phase and carried by a stream of helium gas. The individual CO2 peaks in the helium are subsequently dried in an on-line gas drying unit and admitted to the isotope ratio mass spectrometer via an open split interface.

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Campbell Soup Company

In Move to Expand into Organic Food, Campbell’s Buys Pacific Foods

By Food Safety Tech Staff
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Campbell Soup Company

As consumer preferences continue the shift toward organic food, Campbell Soup Co. announced its $700 million acquisition of Pacific Foods today. The cash deal will help Campbell Soup expand into the organic and functional food spaces, according to company president and CEO Denise Morrison.

“Pacific Foods is an excellent fit with Campbell — strategically, culturally and philosophically,” said Morrison in a company press release. “It advances our strategic imperatives around real food, transparency, sustainability and health and well-being. Culturally, Campbell and Pacific Foods share similar values and a commitment to a purpose-driven approach. Philosophically, both companies believe in making food that we are proud to serve at our own tables using simple, recognizable ingredients.”

Pacific Foods produces organic broth and soup, as well as shelf-stable plant-based beverages and other meals. The Oregon-based company, which employees 540 people, will become part of Campbell’s Americas Simple Meals and Beverages division. Pacific Foods CEO and co-founder Chuck Eggert will remain a supplier of key ingredients through his family farms, which will help the company continue its farm-to-table philosophy. “We’ve spent the past 30 years focused on making nourishing foods with an emphasis on simple, organic ingredients and authentic, rich flavors,” said Eggert. “Looking ahead, a future with Campbell means we can maintain what we value while accelerating growth of the brand in a way that we couldn’t do alone, reaching more people while increasing our impact on sustainable agriculture.”

Randy Fields, Repositrak
FST Soapbox

Update: Non-FSMA Food Safety Litigation

By Randy Fields
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Randy Fields, Repositrak

The keynote panel at the 2017 Food Safety Summit in May had, as any food safety professional would expect, a focus on how companies are coping with FSMA and the increased scrutiny they may face. There was unanimous belief on the panel that enforcement is coming and all trading partners need to be prepared, but there was also a look beyond FSMA adoption to what will come next.

First, though, where do we stand with FSMA-related litigation?

Shawn Stevens, one of the leading food industry lawyers, told attendees that it’s important for all retailers, wholesalers, suppliers and affiliates to understand that FDA was commanded by Congress to stop foodborne illness and the impact it has on Americans, plain and simple. His advice is for food pros to learn all aspects of FSMA and do it quickly, saying the goal now is to avoid making the operational mistakes that may result in criminal exposure for the company and its executive leadership team.

Going forward, the industry will not only have to comply with FSMA, but it will also need to address recalls, risk mitigation and other complex food safety issues not directly related to FSMA. Foodborne illness outbreaks will still cause legal claims that can be compounded by personal injury suits and potentially impact a retailer’s reputation negatively. Also, there are trends in organic foods, GMOs, gluten-free items and more that will impact the retailer, supplier and ultimately may result in more litigation.

Jeffrey Steger, assistant director of the Consumer Division at the U.S. Department of Justice (DOJ), reported that companies shouldn’t expect a waning of the federal government’s support of non-FSMA enforcement actions. The DOJ gets involved in cases where there is significant harm to consumers, where food company executives had prior knowledge, and where legal action will protect the integrity of the regulatory system and prevent future harm. It has pursued many high-profile food industry prosecutions to date and he believes this trend will continue.

The importance of the FSMA regulations and the responsibilities placed on the food industry shouldn’t be understated in the context of food-related litigation. But there are other new developments in the marketplace and the extended supply chain that are impacting retailers like transparency in packaging, labeling of social responsibility programs, the move toward clean labels and facility auditing requirements.

Recent research by the Food Marketing Institute indicates retailers and suppliers that connect with shoppers in support of food safety are well positioned to build shopper trust and loyalty. The converse must also be true—companies that have their reputation dragged down due to involvement in food safety litigation will surely be poorly positioned to build shopper trust and loyalty.

Retailers and suppliers need to address all food safety-related issues or risk becoming defendants in a lawsuit or further government regulation. To accomplish this goal and, more importantly, to keep their customers safe, food companies need to nurture an enterprise-wide food safety culture that extends from the executive suite to store personnel –all retail employees must be responsible for food safety. Only then will customers recognize the company as being committed to food safety, and only then will the company get ahead of any potential food safety-related litigation.

Sudan dye

Adulteration with Sudan Dye Has Triggered Several Spice Recalls

By Thomas Tarantelli
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Sudan dye

In the following article, the author reports finding Sudan dye in spices in New York State, making the argument for Class I recalls.

In New York State (NYS), Department of Agriculture and Markets food inspectors routinely sample domestic and imported food from retail markets for food dye determination. For decades, the NYS Food Lab has examined both domestic and imported food for undeclared allowed food dyes and unallowed food dyes utilizing a paper chromatography method. This method works well with water-soluble acid dyes, of which food dyes are a subset.

The NYS Food Lab has participated in four sets of the FAPAS proficiency tests: Artificial Colours in Soft Drinks and Artificial Colours in Sugar Confectionary (Boiled Sweets). The qualitative analysis was by paper, thin layer silica and thin layer cellulose chromatography. Satisfactory results were obtained.

The paper/thin layer chromatography method is a qualitative non-targeted method and has a limit of detection of approximately 1 to 5 ppm (parts per million) depending on the dye. If an unallowed dye is detected, the food product is violated as adulterated and results are forwarded to the FDA.

Some countries have a maximum concentration of allowed food dye in a food product. For example India has a 100 ppm to 200 ppm maximum for their allowed food dyes, in some food, singly or in combination.1

Sesame seeds, Rhodamine B
Early 2011, sesame seeds were found to contain Rhodamine B.

In early 2011, a food sample of pink colored sugar coated sesame seed from Pakistan was sent to the lab for color determination. The paper chromatography method could not determine any dyes. (As found out later, the unknown pink dye was not an acid dye.) From research it was found that Rhodamine B was a pink water soluble basic dye commonly used as a food adulterant.  A standard was ordered and then a qualitative high performance Liquid chromatography-tandem mass spectrometry (HPLC/MS/MS) method was developed (Waters UPLC Aquity w/Waters Premier XE triple quadrapole) to determine Rhodamine B. After utilizing this new method, Rhodamine B was found in the sugar coated sesame seed.

Rhodamine B is an industrial dye and is not allowed in food anywhere in the world. Industrial dyes are not allowed in food because they are toxic; in fact, some industrial dyes are used for suicide.2,3,4 In addition, industrial dyes are not made to “food grade” specifications with regard to dye purity, heavy metal (i.e., arsenic and lead) concentrations, subsidiary dye concentrations and concentrations of unreacted precursors. From additional research of news articles and research papers, more industrial dyes were identified as common food adulterants; more dye standards were ordered and incorporated into the HPLC/MS/MS method. The NYS Food Lab’s current HPLC/MS/MS surveillance method includes 36 compounds: Water soluble “acid dyes” and “basic dyes”, organic solvent soluble “solvent dyes”, and several pigments.

The HPLC/MS/MS method has a limit of detection in the ppb (parts per billion) range for some dyes and parts per trillion for other dyes. The FDA has an action level of 1 ppb for certain water-soluble basic dyes (such as Malachite Green) when used as a fish antibiotic. However, due to concern that unallowed dyes might be present due to contamination from packaging, the food lab subsequently set an action level of 1 ppm for unallowed dyes determined by the HPLC/MS/MS method. At levels over 1 ppm, detection of dyes in food would indicate intentional dye usage for coloring food.

The food lab has participated in three rounds of the FAPAS proficiency test, “Illegal Dyes found in Hot Pepper Sauce”. The qualitative analysis was by LC/MS/MS. Satisfactory results were obtained.

Sudan Dyes Considered to be Carcinogenic

“Sudan dyes are not allowed to be added to food. There has been worldwide concern about the contamination of chili powder, other spices, and baked foods with Sudan dyes since they may have genotoxic and carcinogenic effects (according to the International Agency for Research on Cancer)”.5

“There have been several documented cases of spices being contaminated with carcinogenic dyes such as Sudan I or lead oxide. We therefore assume that the presence of these chemicals in spice ingredients will be considered a reasonably foreseeable hazard under this rule.”6

“Sudan red dyes have been used to color paprika, chili powders, and curries, but are also known carcinogens and are banned for use in foods.” 7

Sudan Dyes are a family of more than 10 synthetic industrial “solvent dyes”. Solvent dyes are typically used to color oils and waxes, including shoe polish. Sudan dyes that the food lab has found in spices include Sudan 1 (Sudan I), and Sudan 4 (Sudan IV). Sudan 1, also known as Solvent Yellow 14, is an orange colored dye. Sudan 4, also known as Solvent Red 24, is a blue shade red colored dye.

Positive identification of Sudan 4 is often hindered by the existence of a positional isomer, Sudan Red B (Solvent Red 25). This problem was addressed by using the HPLC/MS/MS method with a transition unique to Sudan 4 (381.2 > 276.0). This information was obtained from one of the two corroborating labs. The food lab has recently identified a transition unique to Sudan Red B (381.2 > 366.1).

Sudan Dyes Found in Spices in Europe

In March 2001, Europe began discovering Sudan dyes in spices. A February 2017 search of Europe’s Rapid Alert System for Food and Feed (RASFF) for “unauthorised colour” and “sudan” in the “herbs and spices” food category resulted in 429 notifications.

The 429 RASFF notifications arranged by year and by maximum concentration reported of Sudan 1 and Sudan 4 during that year are listed in Table I.

Sudan dye
Table I.

In a search of the FDA’s Import Alert 45-02 (Detention Without Physical Examination and Guidance of Foods Containing Illegal and/or Undeclared Colors) the author could find no record of spices violated for Sudan dye adulteration.

In a search of the FDA’s Enforcement Reports the author could find no record of spices violated for Sudan dye adulteration.

Industrial Dyes in Food: Class II or Class I Recall?

The NYS Food Lab and the FDA routinely find imported food containing unallowed food dyes such as Ponceau 4R, Amaranth and Carmoisine. These unallowed food dyes are allowed for use in food in other parts of the world, while not allowed in the USA. Foods containing unallowed food dyes are violated as adulterated and a Class II recall will occur. Sudan dyes are not allowed as food dyes anywhere in the world. They are industrial dyes, used in coloring oils and waxes, such as shoe polish.

“Class I recall: A situation in which there is a reasonable probability that the use of or exposure to a violative product will cause serious adverse health consequences or death.

Class II recall: A situation in which use of or exposure to a violative product may cause temporary or medically reversible adverse health consequences or where the probability of serious adverse health consequences is remote.”8

With a Class II recall, there is no consumer notification. In contrast, as part of a Class I recall, a press release is issued. Consumers who have purchased the product might be informed and may discard the product or return it for a refund.

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Minimizing Hazards and Fraud in Milk, IBM Research Partners with Cornell University

By Food Safety Tech Staff
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Americans consume an estimated 600 pounds of milk and milk-based products annually, according to the USDA. In an effort to minimize the hazards in the milk supply and prevent food fraud, IBM Research and Cornell University are joining forces. Combining next-generation sequencing with bioinformatics, the research project will collect genetic data from the microbiome of raw milk samples in a real-world situation at the Cornell University dairy plant and farm in Ithaca, New York.

Specifically, IBM and Cornell will sequence and analyze the DNA and RNA of food microbiomes, which will serve as a raw milk baseline, to develop tools that monitor raw milk and detect abnormalities that could indicate safety hazards and potential fraud. The data collected may also be used to expand existing bioinformatics analytical tools used by the Consortium for Sequencing the Food Supply Chain, a project that was launched by IBM Research and Mars, Inc. at the beginning of 2015.

“As nature’s most perfect food, milk is an excellent model for studying the genetics of food. As a leader in genomics research, the Department of Food Science expects this research collaboration with IBM will lead to exciting opportunities to apply findings to multiple food products in locations worldwide.” – Martin Wiedmann, Gellert Family Professor in Food Safety, Cornell University.

“Characterizing what is ‘normal’ for a food ingredient can better allow the observation of when something goes awry,” said Geraud Dubois, director of the Consortium for Sequencing the Food Supply Chain, IBM Research – Almaden, in a press release. “Detecting unknown anomalies is a challenge in food safety and serious repercussions may arise due to contaminants that may never have been seen in the food supply chain before.”

Cornell University is the first academic institution to join the Consortium for Sequencing the Food Supply Chain.

Ground beef, pink slime

ABC Settles ‘Pink Slime’ Lawsuit with BPI

By Food Safety Tech Staff
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Ground beef, pink slime

Today ABC News and Beef Products, Inc. (BPI) settled the $1 billion+ defamation lawsuit over the television network’s coverage of BPI’s lean finely textured beef, which has been infamously referred to “pink slime”. Terms of the deal are not being disclosed.

“We are extraordinarily pleased with this settlement,” stated BPI attorney Dan Webb in a statement outside the Union County Courthouse in Elk Point, South Dakota, as reported by the Sioux City Journal. “I believe we have totally vindicated the product.”

The ABC reports aired in 2012 (reported by Jim Avila) and stated that ground beef sold in supermarkets contained a cheap filler (beef trimmings sprayed with ammonia) that was not labeled as such on the products. The network reported that 70% of ground beef at the supermarket contained pink slime, a term coined by whistleblower and former USDA scientist Gerald Zirnstein.

BPI claimed that following the ABC reports, its revenues reportedly dropped 80% and resulted in layoffs of hundreds of employees. In a written statement, the company called ABC’s reporting “biased and baseless”. The trial began on June 5.

Clive Longbottom, Quocirca

The Internet of Things: What the Future Holds

By Clive Longbottom
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Clive Longbottom, Quocirca

While the Internet of Things (IoT) is already having a major impact on safety in the food supply chain we’re only just scratching the surface of what connected devices can do to make the industry safer and more efficient. What strikes us as unique and innovative today will likely become standard across the food industry in the years to come as we find new and better ways to apply the technology in all aspects of the business.

One area we can expect to see the impact of the IoT grow is in a broader adoption of automation across the food supply chain. In the context of farming, we’re likely to see autonomous tractors supplant manually driven tractors as the primary equipment used to prepare land. Automated aerial drones will be able to assess the health of crops and deliver highly targeted applications of fertilizers, insecticides and weed killers to cut down on damage caused to crops by excessive use of those products. Transportation, too, is likely to see the impact of automation as driverless trucks take on the majority of shipments of goods.

Another key benefit the IoT will bring to the food industry is improved access to valuable data and in-depth analysis. This will allow more accurate tracking of shipments, better monitoring of quality throughout the supply chain and more useful prediction of potential problems. It’s here that we’re likely to see the biggest impact on pest management, as a broad network of connected sensors will be better able to identify and track pest populations, monitoring their movement and growth in a way that allows pest management professionals to target treatments more effectively. A recent survey of food professionals conducted by Quocirca and commissioned by Rentokil Initial shows that 20% of respondents think IoT will help them deal with cyclical problems such as pest swarms and seasonal flooding, while 19% believe it will provide the most benefit by alerting them to immediate issues such as unexpected pest infestations.

One thing we know for sure is that the technology will become more widely adopted throughout the industry as innovation drives costs down. Initially it will be difficult for smaller organizations with lower margins to invest in cutting edge technology, but as iteration and innovation push the boundaries of what IoT can do, they will also make more basic applications more affordable, as we’ve seen with technology across many industries in recent years.

While it’s easy to speculate and imagine a sci-fi-inspired future of driverless trucks, automated farm machines and limitless access to deep analytics, accurately predicting the exact applications of the IoT as it develops proves more difficult. What we do know is that we can expect the adoption of these technologies to grow at an increasing rate as more innovative and cost effective applications of the IoT are developed.

Deirdre Schlunegger, STOP Foodborne Illness
Food Safety Culture Club

Dave Theno’s Legacy: Keeping People Safe

By Deirdre Schlunegger
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Deirdre Schlunegger, STOP Foodborne Illness

I was putting the finishing touches on this month’s blog post when word came of the tragic and untimely death of Dave Theno, a man whose legacy looms large in the world of food safety.

Just last week I was corresponding with Dave about an honor that STOP Foodborne Illness wanted to bestow upon him at our annual December event that honors our Food Safety Heroes. He had enthusiastically accepted and we were excited to start planning.

Stop Foodborne Illness has a history that is inextricably woven with many of the threads from which Dave’s life was made. In 1993, Dave was called in to help the fast food restaurant Jack in the Box manage the crisis that was the result of an E. coli O157:H7 outbreak, which eventually killed four children and sickened hundreds of others.

At a time when most everyone working in food hadn’t yet realized that food safety was not just another facet of their operation, Dave Theno stood in the gap and helped usher in what has become the modern age of food safety. As he helped industry get on the right track, he also dedicated his life to learning the stories and sharing the pain of families affected by foodborne illness, foremost among them being Roni Rudolph, whose daughter Lauren Beth was the first to die. Together with other hurting parents, Roni founded what would become Stop Foodborne Illness; and in the words of our good friend Mary Heersink, “transformed isolated losses into something bigger than individual tragedy.”

Dave loved his job and did it well. With compassionate integrity and the heart of an advocate, Dave’s strong leadership was proof that he understood the seriousness of the tasks before him. His clear vision for a safer world where food was concerned was a testament to his calling. If there is anything we can learn from Dave Theno’s life, it is that the story is about people. The bottom line is about people. Dave’s compass was considering all the other “Lauren Beths” in the world, and keeping people safe.

He will be sorely missed . . .

Beef ban

USDA Suspends Imports of All Fresh Beef from Brazil

By Food Safety Tech Staff
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Beef ban

Yesterday Sonny Perdue, U.S. Secretary of Agriculture announced that the USDA would be halting all imports of fresh beef from Brazil. The USDA has been inspecting all of the meat products entering the United States from Brazil since March, and has refused entry to 11% of fresh beef products. According to an agency press release, this figure is “substantially higher than the rejection rate of 1% of shipments from the rest of the world”. The increased inspection has resulted in refusal of entry to about 1.9 million pounds of Brazilian beef products over concerns related to public health, sanitary conditions and animal health.

“Although international trade is an important part of what we do at USDA, and Brazil has long been one of our partners, my first priority is to protect American consumers. That’s what we’ve done by halting the import of Brazilian fresh beef.” – Sonny Perdue, U.S. Secretary of Agriculture

The USDA is suspending shipments until the Brazilian Ministry of Agriculture takes corrective action that the agency finds adequate.

David Theno

Swimming Accident Takes Life of Food Safety Expert David Theno

By Food Safety Tech Staff
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David Theno

The news broke this morning that David Theno, one of the most well known experts in the food safety realm, was tragically killed while reportedly snorkeling in Hawaii. He was pronounced dead on Monday following attempts to resuscitate him.

Theno was most notable for his role in implementing new standards in food safety in his position as senior vice president and chief food safety officer at Jack in the Box following the 1993 E. coli O157:H7 outbreak that killed four children. He implemented a HACCP plan and other product testing measures long before it was embraced by many in certain segments of the food industry.

Also a former chief of food safety for Subway, he was in the news over the past week for his testimony in the BPI case versus the ABC network. Theno served as a consultant for BPI from roughly 2010 to 2012, and reportedly reviewed BPI’s food safety practices.

Theno was founder and CEO of his own food safety consulting business, Gray Dog Partners, Inc. He received numerous awards for his outstanding work in food safety during his career, most recently the 2017 NSF Food Safety Leadership Lifetime Achievement Award.