One of China’s and other Asian countries food staples are sweet potato noodles. However, almost 60% of investigated samples tested positive for cassava, a common adulterant in sweet potato noodles (and also the basis for tapioca). The DNA of 52 samples was extracted and analyzed by the real-time loop-mediated isothermal amplification (Real-time LAMP) method, which showed accurate detection down to a 1% limit.
Wang, D., et al. (May 29, 2019). “Detection of Cassava Component in Sweet Potato Noodles by Real-Time Loop-mediated Isothermal Amplification (Real-time LAMP) Method”. Molecules 2019, 24(11), 2043. Retrieved from: doi:10.3390/molecules24112043
Organized crime in Europe has found a new money making machine by engaging in food fraud, which often goes undetected and is relatively low risk compared to other criminal activities. Opson, an Europol-Interpol joint operation, confiscated 16,000 tons of fake food items and 33 million liters of fraudulent beverages in 2018, a new record, but also probably just the tip of the iceberg. Government agencies do not have the resources to detect all fraudulent activities, and suspected food fraud cases moving through the federal and local government hierarchies is a long and cumbersome process.
Food safety and food labeling are strictly regulated in Canada and therefore, honey adulterated with sugars labeled as genuine is considered fraudulent. The Canadian Food Inspection Agency (CFIA) investigated Canadian honey samples from various sources within the supply chain, such as importers, blenders, retailers and more. Almost 22% of imported samples were adulterated with added sugars, the domestic (Canadian) samples showed no adulterations. The CFIA will continue monitoring honey imports and take measures to avoid fraudulent products entering the Canadian market.
Pentobarbital-adulterated products were distributed to pet food manufacturers by a company in spite of receiving a formal notification letter from the FDA. Even a trace amount of this drug makes pet food “adulterated” according to the FDA; in this case the levels of the drug found were quite high. The affected company undertook some corrective measures but was unable to avoid the contamination. However, the company is now supposed to notify the FDA about specific steps regarding sufficient corrective actions within 15 days of receiving the warning letter.
Fresh beef adulterated with sulphur dioxide was found in a Hong Kong market by the Centre of Food Safety. The adulteration of fresh or chilled meat with sulphur dioxide carries hefty penalties of fines and even prison time. Sulphur dioxide is a widely used preservative and antioxidant for foods and beverages that include dried fruits, processed meat products such as sausages, soft drinks and alcoholic beverages. The substance is harmless to healthy persons, however, in subjects with a sulphur dioxide allergy, breathing difficulties and asthma can be induced.
Centre for Food Safety (April 10, 2019). “Fresh beef sample found to contain sulphur dioxide” Centre for Food Safety, The Government of the Hong Kong Special Administrative Region. Accessed April 10, 2019. Retrieved from https://www.cfs.gov.hk/english/press/20190410_7408.html
I attended the Safe Food California Conference last week in Monterey, California. Food fraud was not the main focus of the conference, but there was some good food fraud-related content. Craig Wilson gave a plenary session about the past, present and future of food safety at Costco. As part of that presentation, he discussed their supplier ingredient program. This program was implemented in response to the 2008 Salmonella Typhimurium outbreak in peanut paste but has direct applicability to food fraud prevention.
Food Fraud: Problem Solved? Learn more at the 2019 Food Safety Supply Chain Conference | May 29–30, 2019 | Attend in Rockville, MD or virtually Jeanette Litschewski from SQFI gave a breakout presentation on the most common SQF non-conformities in 2018. She presented data from 7,710 closed audits that cited 44,439 non-conformities. Of those, 756 were related to food fraud requirements. While this presentation was not focused on the specifics of the food fraud non-conformities, Jeanette did mention that many of them were related to broad issues such as not having completed a food fraud vulnerability assessment or appropriately documenting that each of the required factors was addressed in an assessment.
I was invited to give a breakout presentation with an overview of food fraud issues globally and a brief outline of some of the tools currently available to assist with conducting vulnerability assessments. Although many of the attendees had already began implementation of food fraud measures, there was a lot of interest in this list of tools and resources. Therefore, I am recreating the list in Table I. The focus is on resources that are either complimentary or affordable for small- and medium-sized businesses, with recognition that “full-service” and tailored consulting services are always an option.
Of course, there are quite a few companies that offer tailored tools, training and consulting services. Companies that offer courses in food fraud mitigation and assistance in creating a vulnerability assessment (or FDA-required food safety plan) include NSF, Eurofins, AIB International, SGS, and The Acheson Group.
Also available are services that compile food safety recalls and alerts (including those resulting from food fraud) from multiple official sources, such as FoodAKAI and HorizonScan. EMAlert is a proprietary tool that merges public information with user judgment to inform food fraud vulnerability. Horizon Scanning is a system that can monitor emerging issues, including food fraud, globally.
In short, there are many resources available to help support your food fraud vulnerability assessments and mitigation plans. If I have unintentionally missed mentioning any resources you have found to be helpful, please let us know in the comments.
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.
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.
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.).
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.
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.
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
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.
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
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.
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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