FDA has released data from a sampling assignment carried out in 2021 and 2022 to test imported honey for economically motivated adulteration (EMA). EMA can occurs when someone intentionally leaves out, takes out, or substitutes a valuable ingredient or part of a food or when a substance is added to a food to make it appear better or of greater value.

The FDA’s sampling was designed to identify products that contained less expensive undeclared added sweeteners in honey, such as syrups from cane and corn. The agency collected and tested 144 samples of imported honey from bulk and retail shipments from 32 countries and found 14 samples (10%) to be violative. The agency refused entry of violative shipments into the U.S. and placed the associated company and product on an import alert.

FDA routinely assesses imported honey products to ensure accurate product labeling and otherwise help keep consumers from being deceived. The agency will continue to test honey for EMA under the agency’s import sampling and risk-based import entry screening program. Violative samples are subject to agency action, such as recall and import refusal. When appropriate, the agency may consider pursuing criminal investigations. FDA also collaborates with international counterparts to detect and combat EMA related to imported products, including honey.

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On July 12, 2022, FDA issued warning letters to four companies for illegally selling honey-based products that may pose a significant health risk to consumers. The agency’s laboratory testing found that product samples contained active drug ingredients not listed on the product labels, including the active drug ingredients found in Cialis (tadalafil) and Viagra (sildenafil), which are FDA-approved drugs used to treat men with erectile dysfunction and restricted to use under the supervision of a licensed health care professional.

These undeclared ingredients may interact with nitrates found in some prescription drugs, such as nitroglycerin, and may lower blood pressure to dangerous levels.

“Tainted honey-based products like these are dangerous because consumers are likely unaware of the risks associated with the hidden prescription drug ingredients in these products and how they may interact with other drugs and supplements they may take,” said Judy McMeekin, PharmD, FDA associate commissioner for regulatory affairs, in a statement. “Products marketed with unidentified ingredients may be dangerous and, in some cases, deadly to consumers. We encourage consumers to remain vigilant when shopping online or in stores to avoid purchasing products that put their health at risk, and instead seek effective, FDA-approved treatments.”

The warning letters outline how companies violated federal law by selling active drug ingredients in products marketed as foods, such as honey, and by making unauthorized claims that their products treat disease or improve health. These products are promoted and sold for sexual enhancement on various websites and online marketplaces, and possibly in some retail stores. 

The warning letters were issued to:

• Thirstyrun LLC (also known as US Royal Honey LLC);
• MKS Enterprise LLC;
• Shopaax.com; and
• 1am USA Incorporated dba Pleasure Products USA.

Companies marketing food products containing tadalafil and/or sildenafil violate federal law. Some of the products cited in the warning letters are also unapproved new drugs because they are intended for use in the cure, mitigation, treatment, or prevention of disease and they lack FDA approval. Additionally, some products cited in the warning letters are represented as dietary supplements even though tadalafil and sildenafil products are excluded from the dietary supplement definition.

FDA has requested responses from the companies within 15 working days stating how they will address these issues or providing their reasoning and supporting information as to why they think the products are not in violation of the law. Failure to promptly address the violations may result in legal action, including product seizure and/or injunction.

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Food fraud is a significant concern for both consumers and producers. The scale of the problem is significant: 2016 research by Fera Science indicates that fraud accounts for up to 25% of all globally reported food safety incidents. Additionally, growing public demand for food authenticity means that consumers regularly pay a premium price for organic and sustainably produced goods, which is why unprincipled producers and distributors are flooding markets with adulterated, low quality, or mislabeled foodstuffs. This is not only damaging the livelihoods of legitimate businesses, but it’s also risking the health of consumers.

To make matters worse, the potential number of adulterants and the millions of different foodstuffs require a similarly wide range of test methods if food fraud is to be effectively detected and prevented. The rapid growth of global e-commerce also increasingly places food sales outside of regulatory oversight. To catch the food fraudsters, you first need to quickly and efficiently identify their handiwork, which requires special tools.

Assessing Food Authenticity

Analytical testing is an essential technology for assessing food authenticity, which is critical to protect the health of consumers, the food brand, and producer income. Testing is, therefore, a necessary part of an overall strategy to mitigate fraud risk. The techniques and reference databases used for authenticity testing are rapidly evolving, but more still needs to be done, not least in terms of consistency.

There is a lack of adequate testing and test uniformity across the globe. Additionally, many of the test methods reported in the literature either lack applicability to emerging frauds or are simply not deployed in an enforcement framework; however, in recent years, pressure has grown to improve traceability and accountability across the global supply chain, especially for the more commonly adulterated products.

Natural Sweeteners

Current demand for natural sweeteners is high. When consumers purchase a product, they want to be able to recognize the listed ingredients, and know that those ingredients are as natural as possible. This is one of the reasons for increased interest in honey, which has been a natural sweetener for thousands of years. Consumers want more of these natural sweeteners, so the production and sales of honey, particularly organic honey, are experiencing a hefty growth. We’re also seeing that consumers want natural product organic honey, called monofloral honey or unifloral honey, which is basically a honey that comes primarily from a specific type of flower. Consumers are willing to pay more for these products; therefore, we need to protect these consumers by making sure they get what they are paying for.

Creating a Buzz around Honey

One of the most widely adulterated products is the organic variety of honey, a high-value item prized for its unique properties. According to the U.S. Pharmacopeial Convention Food Fraud Database, it’s the third most targeted food for adulteration, after milk and olive oil. It’s also financially significant; a report by Grand View Research valued the global honey market at USD $9.21 billion in 2020 and expects it grow at a compound annual growth rate of 8.2%.

According to data from the United Nations Food and Agriculture Organization, China, Mexico, Russia, Turkey, and the United States are among the major honey-producing countries, accounting for approximately 55% of world production. The most common form of adulteration involves extending or diluting honey with other, less expensive sweeteners, such as corn, cane, and beet syrups. Any form of ingredient addition or substitution that creates a food safety hazard, such as the addition of an unlabeled allergen, must be addressed in the food safety plan.

Therefore, the ability to identify these substances quickly, efficiently, and consistently is essential to tackle fraudulent practices. What the food industry needs is analytical instruments and techniques that can consistently and rapidly fingerprint food and identify trace chemicals.

Setting the Standard

The good news is that liquid chromatography coupled with mass spectrometry (LC-MS) has emerged as the gold standard for analyzing trace constituents in food. The process enables food safety experts to map food components in an unprecedented fashion and will revolutionize how we manage and regulate the quality, safety, and authenticity of food.

While there has been work on developing ways to fingerprint foodstuffs, including honey, approaches among laboratories have varied in terms of sample preparation and analytical methods. There are also differences in terms of data processing. As a result, two laboratories analyzing the same sample could obtain slightly different results. To prevent the problems that may result from these variances, we should be looking at a standardized approach to fingerprinting and analysis.

Refining the Approach

Of course, we are trying to address two issues here: food safety and the quality and authenticity of the product. Each area is governed by separate sets of regulations. If we look at residues of contaminants in honey, such as pesticides, there also are differences between locations. For example, countries can have their own set of restrictions for the maximum limit for specific compounds. When we think about fingerprinting for honey, contaminants are a part of the picture, but the permitted levels vary between countries.

Food authenticity testing utilizing chemical fingerprinting strategies is emerging as a practical approach to tracking food fraud, as chemical fingerprints are virtually impossible to imitate due to their complexity. Regarded as the next-generation surveillance approach for chemicals in food, non-targeted analysis using high-resolution mass spectrometry coupled with innovative software enables the rapid characterization of thousands of chemicals in complex food matrices such as honey.

Currently, samples come from the field to the lab for testing; however, there is interest in potentially reversing this by bringing the lab out into the field. This interesting, but not yet recognized, capability would enable regulators and the food industry to rapidly respond more quickly to honey contamination—and to food fraud in general. By deploying the results of recent fingerprinting research in this way, we will be better equipped to protect consumers and producers alike.

A Global Perspective

The increasing globalization of our food supply chain raises the opportunity for food fraud. Experts predict that testing using methods such as those described above, will become more accessible, increasingly automated, and easier to perform. Fingerprinting methods—in which the entire molecular profile of a food can be obtained—will be a major feature of fraud prevention and identification systems in the future.

The good news is that current testing requirements have led to a rise in rapid, broad-coverage testing methods and technology to enable remote testing of food, in addition to improved testing within laboratory settings. Food testing laboratories can confidently measure contaminants that threaten the global food chain and supply and identify food fraud using these new approaches.

Dr. Bayen is an associate professor in the department of food science and agricultural chemistry at McGill University in Quebec, Canada. He is a recipient of an Agilent Thought Leader Award. Reach him at stephane.bayen@mcgill.ca.

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Honey is a natural food product loved by the global population. However, its limited production, relatively high price, and complex composition make it vulnerable to adulteration. In fact, it ranks in the top 10 most adulterated food products worldwide.

Honey adulteration is a form of food fraud, which is the deliberate and intentional substitution, addition, tampering, or misrepresentation of food, and it’s a major trend impacting the honey industry today.

Wiley has partnered with Agilent Technologies to bring together a special collection of articles detailing the advanced technologies available to detect adulteration and determine the authenticity of honey products. This important compendium features content from Agilent Technologies and Wiley publications, including Food Quality & Safety. In this collection, you’ll read about:

• Detection and estimation of rice syrup in honey;
• Food authenticity testing best practices;
• Preventive measures you can take against food fraud;
• Major honey authentication issues, such as production and origin; and
• Pollen composition, physicochemical parameters, and phenolic and mineral contents of honey samples from Portugal.

We think this series of essential articles will help you combat food fraud in your operations and ensure that your customers are getting a quality product.

Discover this important compendium of content from Agilent Technologies, Food Quality & Safety and Wiley publications. Download the application note to learn more, courtesy of Agilent.

• Application note: Detection and estimation of special marker for rice syrup (SMR) in honey
• Fire up your next food authenticity project
• Food fraud: A criminal activity. Implementing preventative measures that increase difficulty in carrying out the crime
• A comprehensive review on the main honey authentication issues: Production and origin
• Authentication of honeys from Caramulo region (Portugal): Pollen spectrum, physicochemical characteristics, mineral content, and phenolic profile

Download this whitepaper today!

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Throughout history, people have used honey to sweeten and add flavor. Although its sweetness is similar to that of granulated sugar, honey has a distinctive flavor that is largely determined by the flower type from which the nectar is gathered.

According to the Food and Agriculture Organization of the United Nations (FAO), current world honey production is estimated at 1.3 million tons annually.1 The majority of honey produced each year is designated as table honey and intended for direct consumption. The remainder is used as an ingredient in a wide range of products. The food industry uses honey extensively to sweeten and flavor baked goods, cereals, sauces, and beverages. It is also used as a coloring and an emollient in cosmetics such as soap, shampoos, and lotions, as well as in the pharmaceutical industry, primarily to flavor cough remedies and throat lozenges and to soothe and coat the throat.

In total, about 300,000 tons of honey is traded internationally each year. The European Union, the United States, and Japan, which all depend heavily on imported honey to meet consumer demand, together account for 70% of all imports. Given the global patterns that exist in the movement of honey between consuming and producing countries, there is a great international need for analysis to prevent honey that has been contaminated by pesticides, insecticides, or antibiotics from reaching the market.

Environmental contaminants and antibiotics are the most common residues found in honey. For instance, nectar and pollen collected from pesticide-treated flowers can result in contaminated honey. Persistent residues from the antibiotics used to control bacterial diseases in bees can also be a contaminant. Because of extensive honey exporting and importing, analyzing for these contaminants is challenging. One country may approve certain pesticides or antibiotics, while another may ban them. Approved compounds may have varying restrictions on permissible exposure levels.

The Challenge

Increasing concern over the presence of antibiotic and pesticide residues in honey and the related potential health threats to humans has led food quality control laboratories to develop fast and efficient detection methods. The complex honey matrix and the large number and variety of potential contaminants mean that analysis is extremely challenging.

Fundamentally, honey is a highly concentrated solution of two invert sugars, dextrose and levulose, in water with small amounts of numerous complex sugars. In addition to these sugars, which are responsible for the principal physical characteristics and behavior of honey, it also contains aromatic volatile oils, which give it flavor, along with minerals, various enzymes, vitamins, and pigments. These minor constituents, largely responsible for the differences among individual honey types, contribute to the complexity of the honey matrix.

The basic analytical requirements for food analysis are high-resolution, high-throughput, high-sensitivity detection and the quantitation of contaminants at or below the maximum residue limit (MRL) of the compound in a given food matrix.2 Professionals in the food safety and quality control fields recognize liquid chromatography-tandem mass spectrometry (LC-MS/MS) as the central analytical technology. LC-MS/MS provides high-speed, high-resolution, and high-sensitivity separation and quantitation of various chemical compounds. An LC-MS/MS-based technique is also useful as a simultaneous screening method for the multiple classes of contaminants at trace levels in honey.

Honey analysis, like every food analysis, starts with sample preparation. Sample preparation is widely accepted as one of the most critical steps of the LC-MS/MS analysis. The increased demand from food analysis laboratories for higher throughput, higher accuracy, and lower matrix interference has made sample preparation the bottleneck step in the analysis.

Conventional sample preparation for LC-MS/MS analysis of honey is time and labor intensive and often involves pH modification, hydrolysis, liquid-liquid extraction (LLE), solid phase extraction (SPE), solvent evaporation, and pre-concentration steps to isolate and enrich target analytes from the honey matrix. When manually undertaken, these offline techniques are often costly and can result in low sample throughput.

One Solution

Food quality control laboratories are challenged by their need for multi-component quantitation, their desire for limited or no sample preparation, and their requirement to make quality control screening cost effective. New automated, online sample extraction techniques, such as Thermo Scientific TurboFlow technology coupled with LC-MS/MS, can reduce sample preparation and eliminate the disadvantages of conventional techniques.

This new technology allows for direct injection of the honey samples into the MS/MS system, which eliminates time-consuming and costly steps, simplifying the sample preparation process and increasing sample throughput. The technology reduces sample preparation time from hours to minutes and significantly decreases analytical costs. This patented technique also enables automatic removal of proteins and larger molecules from the complex honey mixture. When combined with a triple-stage quadrupole mass spectrometer, efficient quantitative results are possible with reduced levels of ion suppression and chemical noise compared to traditional techniques.

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Representative selected reaction monitoring chromatogram (20 µg/kg) showing the selected ion transitions and retention times for the studied analyte.

Automated online sample extraction technology is based on turbulent flow chromatography, an innovative approach to sample preparation based on chromatographic principles. This process combines principles of diffusion, chemistry, and size exclusion to eliminate matrix interferences while capturing analytes of interest. When the mobile phase flows through the turbulent flow column, high linear velocities are created that are 100 times greater than those typically seen in high-pressure LC columns. This high linear mobile phase velocity and the large interstitial spaces between the column particles create turbulence within the column, which quickly flushes the large sample compounds through the column to waste before they have an opportunity to diffuse into the particle pores, while smaller molecular weight molecules are able to diffuse into the particle pores.

Chemistry also separates analytes from other sample molecules. Those sample molecules that have an affinity to the chemistry inside the pores bind to the column particles’ internal surface. The small sample molecules that have a lower binding affinity quickly diffuse out of the pores and are flushed to waste. A mobile phase change then elutes the small molecules that were bound by the turbulent flow column to the mass spectrometer or to a second analytical column for further separation.

Applications in Screening

A broad, generic, automated LC-MS/MS method has been developed for screening multi-class antibiotics in honey using dual online turbulent flow extraction columns with different chemistries.3 Ten representative antibiotics used in honey, belonging to four different structural classes, were selected: sulfonamides, tetracyclines, aminoglycosides, and macrolides. Sample preparation time was minimal, requiring only the addition of a buffer to reduce sample viscosity. The total LC-MS/MS method run time was less than 18 minutes. This design facilitates the separation and quantification of all of the representative compounds in the complex honey matrix in a single analysis.

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Chromatography comparison of CAP selected reaction monitoring m/z 257 transition (upper traces) and CAP-d5 (lower traces) in pre-blank honey matrix (panel A), at lower limit of quantitation of 0.047 µg/kg (panel B).

For the quantitation of 12 fluoroquinolones and four quinolones in honey, a sensitive and reproducible LC-MS/MS method has been developed.4 An online extraction method using turbulent flow chromatography was employed instead of a traditional SPE method. The sample preparation time decreased from five hours to 40 minutes. The limits of quantitation (LOQ) for the majority of analytes were one µg/kg (parts per billion) with no matrix interference. This online extraction, coupled with a triple-stage quadrupole mass spectrometer, is an excellent total solution for the quantification of a large number of compounds in honey.

A quick, automated sample preparation using the LC-MS/MS method was also developed for the screening of chloramphenicol in honey.5 The only pretreatment required was dilution with water to reduce sample viscosity. The method is sensitive enough to detect 0.023 µg/kg and quantify 0.047 µg/kg of chloramphenicol in honey, significantly lower than the minimum required performance limit of 0.3 µg/kg set by the European Union. Compared to offline detection such as SPE, QuEChERS (quick, easy, cheap, effective, and safe), and LLE, sample preparation with the TurboFlow method was between seven and 24 times faster. The LC-MS method run time was equal to or as much as four times faster than offline detection. Finally, the limit of detection (LOD) was between 5.7 and 20 times lower, and the lower limit of quantitation was between 3.7 and 27 times lower.

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Chromatogram of five fluoroquinolone antibiotic standards at five parts per billion using online clean-up of the Aria TLX-1 system. The system provided a sensitive and reliable analytical method of detecting a full range of antibiotics.

Case Study

The Korea Beekeeping Association (KBA) needed to find an analytical solution that could detect multi-component antibiotics simultaneously and at low levels in honey analysis. They determined that an LC-MS/MS method using a Thermo Scientific Aria system powered by TurboFlow technology was superior to offline sample preparation techniques for antibiotic residue analysis in honey.

The large number and variety of potential contaminants in honey presented a challenge to the KBA. The online sample extraction method on the Aria TLX-1 system provided both increased analysis throughput and higher reproducibility. The system virtually eliminated pre-injection sample preparation, saving labor costs as well as increasing productivity. In addition, matrix effects, which are typically a challenge in LC-MS/MS analysis, decreased. The performance of the method was excellent. The LOD of one ng/mL achieved are well below the maximum residue limits of the antibiotics tested. ■

Ghosh is strategic marketing manager, Food Safety Solutions, Thermo Fisher Scientific. For more information, call (800) 246-4550, e-mail turboflow@thermo.com, or go to www.thermo.com/turboflow.

References

1. Food and Agriculture Organization of the United Nations. FAO Web site. Available at: www.fao.org. Accessed January 26, 2010.
2. 2. Soler C, Mañes J, Picó Y. The role of the liquid chromatography-mass spectrometry in pesticide residue determination in food. Crit Rev Anal Chem. 2008;38(2):93-117.
3. 3. Lafontaine C, Shi Y, Espourteille FA. Multi-class antibiotic screening of honey using online extraction with LC-MS/MS. Thermo Scientific Application Note 464. Available at: www.thermo.com/eThermo/CMA/PDFs/Articles/articlesFile_51570.pdf. Accessed January 26, 2010.
4. 4. Hammel Y-A, Schoutsen F, Martins CPB. Analysis of (fluoro)quinolones in honey with online sample extraction and LC-MS/MS. Thermo Fisher Scientific Application Note 465. Available at: www.thermo.com/eThermo/CMA/PDFs/Articles/articlesFile_51980.pdf. Accessed January 26, 2010.
5. 5. Lafontaine C, Shi Y, Espourteille F. Measurement of chloramphenicol in honey using automated sample preparation with LC-MS/MS. Thermo Scientific Application Note 473. Available at: www.thermo.com/eThermo/CMA/PDFs/Articles/articlesFile_52958.pdf. Accessed January 26, 2010.

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A lone Texas A&M University researcher and a group of North American honey companies and importers are trying to halt the import of mislabeled Chinese honey.

About two years ago, the U.S. government applied tariffs of up to 500% on Chinese honey after exporters began dumping it—selling the honey at a price lower than its cost—in the United States. The dumping practice has seriously undercut the domestic honey market, said Vaughn Bryant, PhD, a palynologist (one who studies spores and pollen) and anthropology professor at Texas A&M University, College Station, Texas.

After the tariffs were put in place, importers noticed something strange: The honey they purchased from countries such as Laos, Cambodia, Vietnam, and Indonesia tasted different than expected. To find out why, they turned to Dr. Bryant, who examines more than 100 pollen sample slides annually, trying to determine the origins of the nectar and honey.

“My analysis pointed out that the reason was [that the honey] wasn’t from those regions. It was from China,” he told Food Quality. In fact, very often the samples he studies “contain all or part Chinese honey.”

Now, in an alleged effort to circumvent the tariffs, Chinese honey is being rerouted through other countries. According to U.S. customs records, millions of pounds of honey are trans-shipped from China to the United States, said Jill Clark of Dutch Gold Honey Inc., in Lancaster, Pa.

Mislabeled honey raises many concerns, especially regarding quality and safety. Clearly, the flavor will be different, Dr. Bryant said. Crystallization speed may differ as well, “which is not good for sales of honey products sitting on grocery shelves,” he said.

Safety can also be an issue. In the past, some Chinese honey has contained antibiotic residues, while other batches have been adulterated, Clark told Food Quality.

Traceability and transparency are problematic, too. “When honey is trans-shipped through another country and its country of origin changes, you lose all ability for traceability and transparency. And people really want to know where their food is coming from,” Clark said.

Honest Honey Initiative

There are several ways to combat the honey problem. Dutch Gold Honey, Golden Heritage Foods LLC, Burleson’s Inc., and Odem International Inc. have launched the Honest Honey Initiative to educate and inform consumers, importers, and producers about illegal honey sales, Clark said. Their first step was unveiling their Website, www.honesthoney.com.

The U.S. government can play a key role in blocking illegal honey imports. The first step is to use accurate labeling. “If you want orange blossom honey and are willing to pay a premium price for it, shouldn’t you actually be getting what you pay for?” Dr. Bryant asked.

Further, a government agency must require the testing of imported honey to confirm country of origin and nectar sources, Dr. Bryant said. “That means the imported honey cannot be filtered,” he said. This is a critical point: Filtered honey contains no pollen; without the pollen, it is nearly impossible to identify origin and nectar sources.

Finally, there must be a standard of identity for honey. “We think this would be one extra step to protect pure and natural honey here in the United States,” Clark said. About three years ago, the industry submitted a citizen’s petition to the U.S. Food and Drug Administration, but the agency has not acted upon it yet. ■

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