In 2004 (another period of high vanilla prices), a company that sourced vanilla beans from Indonesia for use in manufacturing vanilla extract identified mercury contamination in two lots of beans they had received. Mercury was presumably added to increase the weight of the beans. The company quarantined all beans and products that had been manufactured from them. They also had to shut down flavor production to clean and decontaminate the processing equipment.
Due to their high value and physical form (they are often sold in ground or liquid extract form), herbs and spices have a long history of fraudulent adulteration. Many countries have publicly reported being affected by food fraud in herbs and spices over the past 10 years.
Incidents of food fraud reported in the Food Fraud Database for the past ten years in the category “Herbs, Spices, and Seasonings” (68 total).1
Mitigation measures for products at high risk for fraud include putting in place raw material specifications that include authenticity criteria, implementing analytical surveillance, establishing strong supplier relationships and audit programs, and increasing supply chain transparency.
Resource
The Decernis Food Fraud Database is a continuously updated collection of food fraud records curated specifically to support vulnerability assessments. Information is gathered from the scientific literature, regulatory reports, media publications, judicial records, and trade associations from around the world and is searchable by ingredient, adulterant, country, and hazard classification.
Question 1: Is food fraud addressed in the FDA’s Intentional Adulteration rule (“Mitigation Strategies to Protect Food Against Intentional Adulteration”)?
Karen Everstine: Food fraud, or what the FDA calls “economically motivated adulteration” (EMA), is certainly an intentional act. However, recent U.S. regulations for food fraud/EMA are outlined in the Preventive Controls (PC) rules (“Current Good Manufacturing Practice, Hazard Analysis, and Risk-Based Preventive Controls for Human Food” and “Current Good Manufacturing Practice, Hazard Analysis, and Risk-Based Preventive Controls for Food for Animals”) and not in the Intentional Adulteration (IA) Rule. FDA indicated that the IA rule was intended to “prevent acts intended to cause wide-scale harm.” Therefore, new requirements related to food fraud/EMA are included in the hazard analysis requirements in the PC rules. FDA indicated they anticipate EMA preventive controls to be needed only in rare circumstances and “usually in cases where there has been a pattern of EMA in the past.” It is important to note that these requirements are specific to hazards that may be introduced for the purposes of economic gain. EMA that only affects product quality is outside the scope of the PC rules. However, there are misbranding and adulteration provisions of the Food Drug and Cosmetic Act that apply to EMA more broadly (whether or not the substance used may be a hazard).
Question 2: If my facility includes food fraud/EMA in our hazard analysis, will we be compliant with global food fraud requirements?
Everstine: Addressing food fraud/EMA only in your hazard analysis is not sufficient for GFSI compliance. Therefore, if your facility needs to be GFSI compliant, you will need to implement a food fraud vulnerability assessment and mitigation plan that covers all types of fraud. This includes fraud that only affects quality and it includes counterfeiting, theft, diversion, and gray market production. While FDA has indicated they are primarily focused on food fraud/EMA that has a known pattern of occurrence and could be a hazard, GFSI requires that industry evaluate vulnerability more broadly. This includes identifying fraud opportunities (such as complex supply chains), individual capability, and “weak signals” of fraud that could include indicators such as price changes for commodities.
Today Decernis announced that it has acquired USP’s Food Fraud Database. The database was launched in 2012 to assist food manufacturers, retailers and other stakeholders make informed decisions of ingredient vulnerability, food fraud and economically motivated adulteration. It contains information about thousands of ingredients from scientific literature, media publications, regulatory reports, judicial records and trade associations worldwide. Users can use the database to search for information and generate reports.
Decernis and USP will collaborate during the transition process to ensure a seamless integration. Like USP, Decernis is committed to the mission of product safety and we believe the Food Fraud Database has significant runway for expansion through Decernis’ existing platforms, allowing us to scale this important capability and help combat intentional food adulteration,” said Pat Waldo, Decernis CEO.
Priya Rathnam (middle) pictured with Rick Biros, president of Innovative Publishing (left) and Andrew Seaborn Supervisory Consumer Safety Officer, Division of Import Operations, ORA, FDA
How well do you know your suppliers? Can you trust your supplier’s suppliers? What kind of technology are you using to assess and ensure your suppliers are in compliance with regulatory requirements? These are common questions food companies must ask themselves on a regular basis. These and more were addressed at the 2018 Food Safety Supply Chain Conference, held last week at USP in Rockville, MD. Stay tuned for coverage of the event in upcoming articles. In the meantime, here are some top insights shared by FDA and others in industry.
“We’ve issued a limited number of warning letters (two), and they were due to really egregious issues. Where there were previously warning letters issued, we’re seeing a lot more ‘regulatory meetings’.” – Priya Rathnam, Supervisory Consumer Safety Officer, CFSAN, on FDA’s enforcement this fiscal year.
Criteria for FSMA auditors also includes the “soft skills”, aka ISO 19011, auditor personal attributes. –Josh Grauso, Senior Manager, Food Safety & Quality System Audits, UL
Food fraud costs the industry up to $15 billion annually. – Fabien Robert, Ph.D., Director, Nestle Zone America
It’s concerning that so many QA managers (and other pros) today don’t know extent of risk assessment they need to carry out. – Chris Domenico, Safefood360, Territory Manager for North America
“Blockchain is more than a buzzword at the moment.”- Simon Batters, Vice President of Technology Solutions, Lloyd’s Register
A dynamic panel about blockchain, led by Darin Detwiler, Director: Regulatory Affairs of Food and Food Industry, Northeastern University featured (left to right) Kathy Wybourn, Director, Food Safety Solutions, DNV Business Assurance; Simon Batters,Vice President of Technology Solutions, Lloyd’s Register and Melanie Nuce, Senior Vice President, Corporate Development & Innovation, GS1 US.
Sometimes food safety doesn’t win; sometimes you need the business acumen to show that implementing supply chain efficiencies will create the win. – Gina Kramer, Executive Director, Savour Food Safety International
Building a robust & smart supply chain = reduce food miles, shrink carbon footprint, and save food waste to increase revenue/acre. – Bryan Cohn, Vice President of Operations, Seal the Seasons
The FSMA Sanitary transportation rule is not as straightforward as you think. We need more training. – Cathy Crawford, President, HACCP Consulting Group
In a two-question format, the authors discuss pressing issues in food fraud.
1. Where are the current hot spots for food fraud?
Food fraud activities have been known for centuries. For example, in ancient Rome and Athens, there were rules regarding the adulteration of wines with flavors and colors. In mid-13th century England, there were guidelines prescribing a certain size and weight for each type of bread, as well as required ingredients and how much it should cost. In the United States, back in 1906, Congress passed both the Meat Inspection Act and the original Food and Drugs Act, prohibiting the manufacture and interstate shipment of adulterated and misbranded foods and drugs. However, evidence and records of actions taken over those events were not officially collected.
It was not until 1985, when the presence of diethylene glycol (DEG) was identified in white wines from Austria, that authorities, retailers and consumers started to have serious concerns about the adulteration of food and the severity of its impact on consumers. In addition, there was increased interest to regulate, investigate and apply efforts to enforce requirements.
Other examples include the following:
2005: Chili powder adulterated with Sudan (India)
2008: Dairy products adulterated with melamine (China)
2013: Beef substituted with horsemeat (UK)
2013: Manuka honey where it was known that bees were not feeding from pollen of the Manuka bush (New Zealand)
2016: Dried oregano adulterated with other dried plants (Australia)
This list can go on and on.
Lately there have been more cases of food fraud. Fortunately, even limited international databases are helping to identify the raw material origins of products in the supply chain that could be more exposed to adulteration. Also, food manufacturers, brokers and agents are conducting assessments to ensure that they are buying ingredients and products from sources, where food fraud could be prevented. The following products are identified as having more adulteration notifications:
Olive oil
Fish
Vegetable products with claims of “Organic”
Milk
Grains
Honey and maple syrup
Coffee and tea
Spices
Wine
Fruit Juices
2. What can companies do to mitigate the risk?
Control measures to prevent food fraud activities include the adequate evaluation and selection of suppliers, as well as the ‘suppliers of the suppliers’. Typical risk matrices of likelihood of occurrence versus consequence can be used to measure risk—and determine priorities for assessing and putting control measures in place. Assessments can be focused on points of vulnerabilities such as food substitution, mislabeling, adulterations and/or counterfeiting, usually due to economic advantages for one or more tiers in food chain production.
Other food fraud activities include effective traceability systems, monitoring current worldwide news and notifications on food fraud using international databases (EU-RASFF, USA- EMA NCFPD and USP, etc.), and product testing.
Product testing is becoming an important tool for the food industry to become confident in sourcing raw materials, ensuring the management of food fraud control measures, fulfilling applicable legal requirements, and ensuring the safety of consumers.
Product testing laboratories offer different kinds of testing methods depending on the required output; for example, if it is possible and requested, a targeted or non-targeted result.
Targeted analysis involves screening for pre-defined components in a sample:
Liquid chromatography
Gas chromatography
Mass spectrometry (LC-MS and GC-MS)
Nuclear magnetic resonance spectroscopy (NMR).
PCR technique
Non-targeted analysis aims to see any chemical present in the sample:
Isotopic measurement-determination of whether ethanol and vinegar and flavorings are natural or synthetic
Metabolomics: Maturation and shelf life
Proteomics: Testing for pork and beef additives in chicken, confectionery and desserts
Due to the importance of food fraud for a food safety management system, GFSI published Version 7.1 of Benchmarking Requirements, including subjects on food fraud, as vulnerability assessment. In 2018 all certification schemes have incorporated such requirements and started enforcing them.
Fraud cases threat consumer trust in products and services. Companies are learning to “think like a criminal” and put in place measures to prevent fraud and protect their products, their brands and their consumers.
Laboratory reports recently acquired by the Freedom of Information Law from the New York State Department of Agriculture and Markets show the Sol Andino brand ground cumin to contain 1090 ppm lead as well as 259 ppm chromium. The spice was also analyzed by IS:2446, 1980 method, “Detection of Lead Chromate in Chillies, Curry Powder and Turmeric by diphenyl carbizide.” A positive result was given, indicating the presence of hexavalent chromium, which is a component of lead chromate. Lead chromate is a yellow pigment, not allowed in food anywhere in the world as it is toxic, containing both lead and hexavalent chromium. The New York State Department of Agriculture and Markets posted a Class I recall of the Sol Andino ground cumin on July 10, 2017, without mention of the extremely high concentration of lead in the product.
Sol Andino ground cumin recalled
The author could find no record of an FDA recall for the Sol Andino brand cumin powder containing excessive lead.
Some of us remember the four FDA Class I recalls of Pran brand turmeric for excessive lead in October 2013. These recalls were initiated by the New York State Health Department due to an illness complaint—most likely a child with high blood lead levels. The recalled Pran brand turmeric contained 28–53 ppm lead.
“There have been two cases of high blood levels of lead associated with this product to date. Both cases have been reported through the Illinois Department of Public Health, Environmental Health Protection.”
According to the recall, the “Thyme” was found to contain 422 ppm lead.
Wondering if the 422 ppm lead was caused by adulteration of the “Thyme” with lead chromate or another lead pigment, a food chemist at the New York State Food Laboratory (a Division of NYS Dept. of Agriculture and Markets) requested from Illinois a sub-sample of the “Thyme” for analysis. Lab analysis of the spice found 323 ppm lead, 109 ppm chromium and a positive result for the chromate test. Thus, this recalled “Thyme” contains lead chromate.
In both cases, Pran turmeric and Nabelsi Thyme, illness complaints led to the recall of lead adulterated spices.
The New York State Department of Agriculture and Markets has a proactive program. Random samples of spices are sampled from retail markets and subsequently analyzed for unallowed colorants, undeclared allergens and heavy metals. In 2016 this resulted in the Oriental Packing Class I recall of 377,000 lb. of turmeric containing spices for excessive lead. (A typo in the FDA recall attributes the recall to the New York State Health Department, instead of the New York State Dept. of Agriculture and Markets.)
Still, it’s even better to analyze spices being imported into the country at receiving warehouses before the product reaches retail markets. Lead concentrations above 10 ppm can be determined instantaneously with a handheld XRF analyzer.
The World Factbook of Food is a central reference location for data related for food. (Click to enlarge image of homepage)
Many foods, from honey to olive oil to spices, fall victim to fraudsters each year. Often a time-consuming process, conducting research about each product or ingredient can involve combing through many websites and databases for information. To save companies from doing all that heavy lifting, newer tools are aggregating the data into single platforms. One most recent example is the World Factbook of Food, developed by the Food Protection and Defense Institute (FPDI) and funded by the U.S. Department of Homeland Security. The tool was released earlier this year, and Erin Mann, project manager at FPDI, explains how it is helping food companies mitigate the risk of food fraud in their supply chain.
Food Safety Tech: What are the fundamental advantages of using the World Factbook of Food and how is it different from other tools that companies can use to assess their risk?
Erin Mann: The World Factbook of Food is a central reference location for data related for food. It pulls together a lot of high quality data points from a lot of different sources into a single tool.
Companies can look for information on a lot of different food products and a lot of different sourcing regions and countries. We have more than 125 food profiles (and growing) and more than 75 country profiles (also growing). [There are 10 food profiles and 10 country profiles that are available for free] Each of the profiles covers a large number of topics. On the food profile side, there are data points on how the product is used, codes, information about standards and grades; and a lot of data about trends and consumption, production and trade patterns; there’s information about processing and supply chain characteristics; and another section about food defense and food safety.
Erin Mann, Food Protection and Defense Institute
It’s a resource that can be used anytime a company needs to get up to speed quickly on a product, because it covers a lot of different types of risks. If a company wanted access to information related to risk about past economically motivated adulteration (EMA) or intentional adulteration (IA) incidents, the Factbook has that. There’s also data on past recalls, information about major producing countries around the world—a wealth of information in one place that companies can use broadly for risk assessment—basically any use case where they want access to a lot of information from lots of sources, the Factbook can be a great place for that.
FST: Can you expand on the food defense component of the Factbook?
Mann: One of the primary sources that we pull for the food defense section comes from a complementary tool that we use here at FPDI—our food adulteration incidence registry, called the FAIR tool, which is a database of past EMA and IA incidents. On the technology side, the Factbook is directly linked with the FAIR tool. If you’re looking at a profile for a particular product, it will access the FAIR tool and display relevant incidents for that product. It won’t give you access to the entire FAIR database, but it will give you a high-level summary of what food defense incidents have happened in the past with the product, where they happened, the year and a summary.
What we’ve seen with the FAIR tool is high incidents of food adulteration in products like oils, spices, seafood—those are the major products impacted by food adulteration, particularly EMA.
Food Adulteration Incidents Registry (FAIR) tool
FST: From what sources are the data curated?
Mann: There’s a source list at the bottom of each profile and all the data points are referenced throughout. In terms of a high-level description of where we pull data from, it includes the USDA, FDA, Codex, the U.S. International Trade commission, United Nations data, and other industry and trade groups. It also pulls data from the World Bank and the FAIR tool.
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FST: How can companies use the Factbook as part of their overall risk mitigation process?
Mann: One of primary strengths of the Factbook is that companies can use it in many different ways. Our institute has done a lot of work with big data and using multiple data sources, and one of the biggest takeaways we learned through several years in this field is that whenever you use big data or you use lots of data sources, they must produce intelligence and information that is actionable. All of the data and information doesn’t do much good if there’s not a clear summary of what to do with that information.
The Factbook aims to do that. It’s a collection and synthesis of data and clean information that’s in an easy to use and easy to navigate user interface. From there, companies can take a look and see how to use the Factbook where they see a gap in their processes. It’s a great place to access lots of information about a food product in a single place. If we can see several points in an overall risk mitigation process where the Factbook can be used, it could be used to inform decisions related to procurement. [For example], if a company suddenly needed to procure a product from a new source region or if they were developing a new product and had to procure an ingredient that they hadn’t worked with before, the Factbook would be a great place to get smart quickly on that ingredient.
The Factbook could be used for understanding supplier review and specific risks related to that ingredient, or simply horizon scanning—if companies want to take a look at some of the products they’ve determined to be high risk and learn more about the product from a holistic perspective.
As stated in the Q&A, 10 food profiles and 10 country profiles are available for free. Subscribers to the World Factbook of Food pay $600 annually for full access to the tool, and bundled pricing is available for users who are interested in access to both the Factbook and the FAIR tool.
Food defense is the protection of food products from intentional contamination or adulteration, as well as biological, chemical, physical or radiological agents. It addresses additional concerns including physical, personnel and operational security. A traditional food defense program is generally perceived as a program that includes site security, visitors control or even on-site personnel monitoring. However, with the new FSMA Preventive Controls Rules and GFSI Guidance for all the recognized schemes, additional to consumer demand on product transparency, we must now take food fraud into consideration within our food defense program.
What is food fraud? According to the study from Michigan State University, 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 misleading statements made about a product, for economic gain. It becomes not just a potential for food safety issues, but also a severe issue that could potentially damage your brand reputation. It is hence critical to have appropriate protection and prevention, as the umbrella encompasses both food defense and food safety.
What does this mean to food manufacturers? The awareness of traceability and transparency certainly should rise. Most facilities should have a food defense program in place to comply with any GMP or GFSI requirements. To make it more competent for food fraud, what could we do? Here are some quick tips to strengthen your food defense program with food fraud prevention:
Tip 1: Review your entire supply chain one more time, considering fraud risks
Tip 2: Use the HACCP concept for food fraud risk analysis
Tip 3: Double-check incoming goods
Tip 4: Make the entire supply chain transparent
Tip 5: Document all records
Tip 1: Review your entire supply chain one more time, considering fraud risks
The unknown could potentially hurt you or your program. You would prefer to be aware of what might go wrong before it goes wrong, which is why a review should be one of the key steps in your food safety program. It might be a familiar terminology in the industry; however, we could not eliminate its importance to your entire food safety management system. To maintain product authenticity, understanding where your ingredients come from and who your business partners and suppliers are become the first step to success. It also gives you an excellent opportunity to analyze the risks and potential risk sources. A thorough review should include all the approved suppliers and vendor information. Knowing the source of your product provides you with a good foundation for your food defense program. How can we efficiently review our own supply chain?
List all approved suppliers and contract vendors
Make sure all ingredients are used accordingly and as intended
Keep the supplier registration list up to date
The more you understand your own supply chain, the more helpful it will be to your food defense program.
Tip 2: Use HACCP concept for food fraud risk analysis within supply chain
Hazard Analysis Critical Control Point (HACCP), as defined by FDA, is a management system in which food safety is ensured by addressing through the analysis and control of biological, chemical and physical hazards throughout the entire supply chain. This mentality of HACCP could be used and very helpful to analyze the potential fraud risks. Its seven principles and 12 steps could be implemented to identify your own fraud risks. And it is important for us to identify the hazards from potentially adulterated ingredients to determine the next step for what needs to be controlled. Utilizing the 12 steps, we can list all the key points and steps that could potentially impact your products’ authenticity. The risks can come from personnel, visitors or the ingredients themselves. There are many resources out there; for example, US Pharmacopeia (USP) has developed a global food fraud database that is a good resource for all ingredients that have been falsely used in food products.
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Tip 3: Double-check incoming goods
Many articles address the importance of vulnerability assessments to prevent food fraud plus any documentation your suppliers have provided. Yes, it is critical; however, as one of the important steps in the HACCP program, verification is also important to make sure what goes into your finished products is safe and guaranteed. This could be addressed and monitored by implementing genetic testing. Each product and ingredient has its own DNA, just like our fingerprints. Nowadays, there are many methodologies developed for this type of test. The DNA testing could be a helpful tool to help your facility verify the authenticity of your incoming raw materials. Genetic testing using techniques like polymerase chain reaction (PCR) technology to detect the DNA of the product upon receiving the incoming goods. Moreover, as fast as it can be, facilities can now receive the test results within one to two hours. The testing itself might seem like an extra step with more effort and labor. However, the return is a huge saving on damages caused by food fraud. You can now start to verify and control your supply chain from the beginning to avoid any potential adulteration.
Tip 4: Make the entire supply chain transparent
This transparency not only applies to internal employees but also outward to your customers and vendors. That way you can familiarize yourself with your own supply chain, while at the same time establish brand reputation and confidence to your customers.
Tip 5: Keep all records documented
The records you should keep, besides a registration list of all your ingredients and vendors, should include the inventory list, how ingredients are used, whether it is used outside of its intended use and authorized personnel signatures. The following are some tips for an efficient document control:
Make it clear and straightforward
Categorize it based on your own facility operations
Keep the records in the same order of your supply chain from ingredients to end consumers
After all, with the newly released requirements, as QA professionals, we need to start developing a mindset that considers food fraud as a type of hazard, and develop monitor and control strategies for mitigating it. Just like we are now so familiar with the physical, chemical and biological hazards within our production facilities compared to decades ago, food fraud will no longer be a scary term once it is proficiently understood and properly controlled.
Food fraud is a recognized threat to the quality of food ingredients and finished food products. There are also instances where food fraud presents a safety risk to consumers, such as when perpetrators add hazardous substances to foods (e.g., melamine in milk, industrial dyes in spices, known allergens, etc.).
FSMA’s Preventive Controls Rules require food manufacturers to identify and evaluate all “known or reasonably foreseeable hazards” related to foods produced at their facilities to determine if any hazards require a preventive control. The rules apply both to adulterants that are unintentionally occurring and those that may be intentionally added for economically motivated or fraudulent purposes. The FDA HARPC Draft Guidance for Industry includes, in Appendix 1, tables of “Potential Hazards for Foods and Processes.” As noted during the recent GMA Science Forum, FDA investigators conducting Preventive Controls inspections are using Appendix 1 “extensively.”
The tables in Appendix 1 include 17 food categories and are presented in three series:
Information that you should consider for potential food-related biological hazards
Information that you should consider for potential food-related chemical hazards
Information that you should consider for potential process-related hazards
According to the FDA draft guidance, chemical hazards can include undeclared allergens, drug residues, heavy metals, industrial chemicals, mycotoxins/natural toxins, pesticides, unapproved colors and additives, and radiological hazards.
USP develops tools and resources that help ensure the quality and authenticity of food ingredients and, by extension, manufactured food products. More importantly, however, these same resources can help ensure the safety of food products by reducing the risk of fraudulent adulteration with hazardous substances.
Geographic Distribution of Incidents for Dairy Ingredients. Graphic courtesy of USP.
Data from food fraud records from sources such as USP’s Food Fraud Database (USP FFD) contain important information related to potential chemical hazards and should be incorporated into manufacturers’ hazard analyses. USP FFD currently has data directly related to the identification of six of the chemical hazards identified by FDA: Undeclared allergens, drug residues, heavy metals, industrial chemicals, pesticides, and unapproved colors and additives. The following are some examples of information found in food fraud records for these chemical hazards.
Undeclared allergens: In addition to the widely publicized incident of peanuts in cumin, peanut products can be fraudulently added to a variety of food ingredients, including ground hazelnuts, olive oils, ground almonds, and milk powder. There have also been reports of the presence of cow’s milk protein in coconut-based beverages.
Drug residues:Seafood and honey have repeatedly been fraudulently adulterated with antibiotics that are not permitted for use in foods. Recently, beef pet food adulterated with pentobarbital was recalled in the United States.
Heavy metals:Lead, often in the form of lead chromate or lead oxide which add color to spices, is a persistent problem in the industry, particularly with turmeric.
Industrial Chemicals: Industrial dyes have been associated with a variety of food products, including palm oil, chili powder, curry sauce, and soft drinks. Melamine was added to both milk and wheat gluten to fraudulently increase the apparent protein content and industrial grade soybean oil sold as food-grade oil caused the deaths of thousands of turkeys.
Pesticides: Fraud in organic labeling has been in the news recently. Also concerning is the detection of illegal pesticides in foods such as oregano due to fraudulent substitution with myrtle or olive leaves.
Unapproved colors/additives: Examples include undeclared sulfites in unrefined cane sugar and ginger, food dyes in wine, and tartrazine (Yellow No. 5) in tea powder.
Time Series Plot of Records for Chili Powder (blue), Skim Milk Powder (green), and Olive Oil (orange)
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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If you disable this cookie, we will not be able to save your preferences. This means that every time you visit this website you will need to enable or disable cookies again.
Cookie Policy
A browser cookie is a small piece of data that is stored on your device to help websites and mobile apps remember things about you. Other technologies, including Web storage and identifiers associated with your device, may be used for similar purposes. In this policy, we say “cookies” to discuss all of these technologies.
Our Privacy Policy explains how we collect and use information from and about you when you use This website and certain other Innovative Publishing Co LLC services. This policy explains more about how we use cookies and your related choices.
How We Use Cookies
Data generated from cookies and other behavioral tracking technology is not made available to any outside parties, and is only used in the aggregate to make editorial decisions for the websites. Most browsers are initially set up to accept cookies, but you can reset your browser to refuse all cookies or to indicate when a cookie is being sent by visiting this Cookies Policy page. If your cookies are disabled in the browser, neither the tracking cookie nor the preference cookie is set, and you are in effect opted-out.
In other cases, our advertisers request to use third-party tracking to verify our ad delivery, or to remarket their products and/or services to you on other websites. You may opt-out of these tracking pixels by adjusting the Do Not Track settings in your browser, or by visiting the Network Advertising Initiative Opt Out page.
You have control over whether, how, and when cookies and other tracking technologies are installed on your devices. Although each browser is different, most browsers enable their users to access and edit their cookie preferences in their browser settings. The rejection or disabling of some cookies may impact certain features of the site or to cause some of the website’s services not to function properly.
Individuals may opt-out of 3rd Party Cookies used on IPC websites by adjusting your cookie preferences through this Cookie Preferences tool, or by setting web browser settings to refuse cookies and similar tracking mechanisms. Please note that web browsers operate using different identifiers. As such, you must adjust your settings in each web browser and for each computer or device on which you would like to opt-out on. Further, if you simply delete your cookies, you will need to remove cookies from your device after every visit to the websites. You may download a browser plugin that will help you maintain your opt-out choices by visiting www.aboutads.info/pmc. You may block cookies entirely by disabling cookie use in your browser or by setting your browser to ask for your permission before setting a cookie. Blocking cookies entirely may cause some websites to work incorrectly or less effectively.
The use of online tracking mechanisms by third parties is subject to those third parties’ own privacy policies, and not this Policy. If you prefer to prevent third parties from setting and accessing cookies on your computer, you may set your browser to block all cookies. Additionally, you may remove yourself from the targeted advertising of companies within the Network Advertising Initiative by opting out here, or of companies participating in the Digital Advertising Alliance program by opting out here.
