Tag Archives: analysis

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Hot on Food Fraudsters’ Heels

By Susanne Kuehne
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Susanne Kuehne, Decernis
Microscope, pepper
Find records of fraud such as those discussed in this column and more in the Food Fraud Database. Image credit Susanne Kuehne.

The Institute of Global Food Security at Queen’s University Belfast successfully identifies food fraud in the ever more complex food supply chain by developing and applying reliable analytical tests. Chris Elliott, professor of food safety and founder of the Institute, points out a two-tier approach of untargeted analysis and targeted analysis. Tier One is low cost and easy-to-use with 80–90% reliability. The second tier of highly sophisticated analytical methods, like mass spectrometry, gas chromatography and others, can identify a food item with a 99.999% certainty. These analytical methods combined with correct data are able to identify even details like type of fish, country of origin of a food item, added ingredients, and much more.

Resource

  1. Professor Chris Elliott. (August 13, 2020). “Reliable targeted analysis solutions to fight food fraud.” The Scientists’ Channel.
Susanne Kuehne, Decernis
Food Fraud Quick Bites

The Very Mellow Yellow

By Susanne Kuehne
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Susanne Kuehne, Decernis
Adulteration
Find records of fraud such as those discussed in this column and more in the Food Fraud Database. Image credit Susanne Kuehne.

Lead chromate, flour, curcuma, Metanil Yellow or Sudan Dye, anyone? These are just some of the possibly hazardous adulterants that may make their appearance in turmeric, a popular and pricey spice and ingredient in dietary supplements. The American Botanical Council published a laboratory guidance document to determine the proper methods for the analysis of a number of adulterants. The document gives lists of the methods with their pros and cons, grouped by type of adulterant.

Resource

  1. Cardellina II, J.H., Ph.D. (2020). “Turmeric Raw Material and Products Laboratory Guidance Document”. American Botanical Council.
Vitamins

Revamped Liquid Chromatography Enhances Analysis of Vitamins and Beyond

By Maria Grübner
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Vitamins

Vitamins play a critical role in the regulation of key physiological processes, such as blood clotting, metabolism and maintaining our vision. These biologically important compounds can be divided into two broad classes based on their solubility and differ in the way they are handled in the body—and in food safety laboratories. While excess amounts of water-soluble vitamins (including B1, B2, B3, B6 and B12) are excreted, fat-soluble vitamins (including vitamin A, D, E and K) can be stored in the liver or fatty tissue for later use. The simultaneous analysis of water- and fat-soluble vitamins in traditional liquid chromatography is difficult, and is compounded by the presence of biologically important vitamin isomers, which exist at lower concentrations and demand greater sensitivity from analytical techniques.

Food analysis laboratories support food manufacturers by assessing food safety and authenticity, and have a responsibility to produce precise and reliable data. Vitamins are among a number of compounds assessed in infant formulas, energy drinks and other supplements, and are added to fortify the nutritional value of these products. Given the critical nutritional role of vitamins, especially during early developmental periods, their characterization is highly important. This, along with the challenging and cumbersome nature of vitamin analysis, has spurred the development of innovative high-performance liquid chromatography (HPLC) methods for food safety testing.

Unique Challenges of Vitamin Analysis

The simultaneous analysis of water- and fat-soluble vitamins is difficult to achieve with reversed-phase high-performance liquid chromatography, due to the wide range of hydrophobicity among vitamins. Highly hydrophobic fat-soluble vitamins are retained strongly by chromatography columns and are only eluted with high-strength mobile phases. In contrast, water-soluble vitamins are usually poorly retained, even with very weak mobile phases. As the ideal conditions for chromatographic separation are very different for the two vitamin classes, there have been efforts to explore the possibility of operating two columns sequentially in one system. The early versions of this approach, however, were not well suited to high-throughput food safety laboratories, requiring complex hardware setup and even more complicated chromatography data system programming.

Prior to liquid chromatography analysis, food samples must be purified and concentrated to ensure target analytes can be detected without matrix interference. Liquid-liquid extraction is one purification method used to prepare for the analysis of vitamins and other compounds; it was one of the first methods developed for purification and enables compounds to be separated based on their relative solubilities in two different immiscible liquids.1 It is a simple, flexible and affordable method, yet has several major disadvantages.2 Liquid-liquid extraction consists of multiple tedious steps and requires the use of large volumes, therefore the time for completion is highly dependent on the operator’s skills and experience. Consequently, the duration of sample exposure to unfavorable conditions can vary greatly, which compromises reproducibility and efficiency of the method. This is of concern for vitamins that are particularly prone to degradation and loss when exposed to heat and light, such as vitamin D in milk powder.

Two-Dimensional Liquid Chromatography Enables Deeper and Faster Analysis

Analysts in the food industry are under pressure to process high volumes of samples, and require simple, high-throughput and high-resolution systems. Fortunately, two-dimensional liquid chromatography (2D-LC) systems have evolved markedly in recent years, and are ideally suited for the separation of vitamins and other compounds in food and beverages. There are two main types of systems, known as comprehensive and heart-cutting 2D-LC. In comprehensive 2D-LC, the sample is separated on the first column, as it would be in 1D-LC. The entire eluate is then passed in distinct portions into a second column with a different selectivity, enabling improved separation of closely eluting compounds. In contrast, heart-cutting 2D-LC is more suited to targeted studies as only a selected fraction (heart-cut) of the eluate is transferred to the second-dimension column.

Recently, another novel approach has emerged which utilizes two independent LC flow paths. In dual workflows, each sample is processed by two columns in parallel, which are integrated in a single instrument for ease of use. The columns may offer identical or different analyses to enable a higher throughput or deeper insights on each sample. This approach is highly suited to vitamin analysis, as the two reversed-phase columns enable simultaneous analysis of water- and fat-soluble vitamins. A simple, optimized preparation method is required for each of the two vitamin classes to ensure samples are appropriately filtered and concentrated or diluted, depending on the expected amount of analyte in the sample. The dual approach enables a broad range of ingredients to be assessed concurrently in supplement tablets, energy drinks, and other food and beverages containing both water- and fat-soluble vitamins. For analysts working to validate claims by food vendors, these advances are a welcome change.

Refined Detection and Extraction Methods Create a Boost in Productivity

Analysts in food analysis laboratories now have a better ability to detect a wide range of components in less time, due to improved detection and extraction methods. Modern LC systems utilize a wide range of analytical detectors, including:

  • Mass spectrometry (MS)
  • Diode array detection (DAD)
  • Multi-wavelength detection
  • Charged aerosol detection (CAD)
  • Fluorescence detection (FLD)

The optimal detector technology will depend on the molecular characteristics of the target analyte. Infant formula, for example, can be analyzed by DAD and FLD, with detection and separation powerful enough to accurately quantify the four isomers of vitamin E, and separate vitamin D2 and D3. Highly sensitive 2D-LC methods are also particularly favorable for the trace level quantitation of toxins in food, such as aflatoxins in nuts, grains and spices.

Given the limitations of liquid-liquid extraction, an alternative, simplified approach has been sought for 2D-LC analysis. Liquid-liquid extraction, prior to chromatography analysis, involves many tedious separation steps. In contrast, the use of solid phase extraction for infant formula testing reduces pre-treatment time from three hours to one hour, while improving detection. This is of great significance in the context of enterprise product quality control, where a faster, simpler pre-treatment method translates into a greater capacity of product testing and evaluation.

HPLC Toolkit for Food Safety Analysis Continues to Expand

Several other HPLC approaches have also been utilized in the field of food safety and authentication. For example, ultra-high-performance liquid chromatography (UHPLC) with detection by CAD followed by principal component analysis (PCA) can be used to investigate olive oil purity. In contrast to conventional approaches (fatty acid and sterol analysis), this revised method requires very little time and laboratory resources to complete, enabling companies to significantly reduce costs by implementing in-house purity analysis. With a reduced need for chemicals and solvents compared with fatty acid and sterol analyses, UHPLC-CAD provides a more environmentally friendly alternative.

Analyzing amino acid content in wine is an important aspect of quality control yet requiring derivatization to improve retention and separation of highly hydrophilic amino acids. Derivatization, however, is labor-intensive, error-prone, and involves the handling of toxic chemicals. To overcome these limitations, hydrophilic interaction liquid chromatography (HILIC) combined with mass detection has been identified as an alternative method. While HILIC is an effective technique for the separation of small polar compounds on polar stationary phases, there still may be cases where analytes in complex samples will not be completely separated. The combination of HILIC with MS detection overcomes this challenge, as MS provides another level of selectivity. Modern single quadrupole mass detectors are easy to operate and control, so even users without in-depth MS expertise can enjoy improved accuracy and reproducibility, while skipping derivatization steps.

Conclusion

Recent innovations in 2D- and dual LC technology are well suited to routine vitamin analysis, and the assessment of other components important in food safety evaluation. The concurrent and precise assessment of water- and fat-soluble vitamins, despite their markedly different retention and elution characteristics, is a major step forward for the industry. Drastic improvements in 2D-LC usability, flexibility and sensitivity also allows for biologically important vitamin isomers to be detected at trace levels. A shift towards simpler, high-throughput systems that eliminate complicated assembly processes, derivatization and liquid-liquid extraction saves time and money, while enabling laboratories to produce more reliable results for food manufacturers. In terms of time and solvent savings, solid phase extraction is superior to liquid-liquid extraction and is one of many welcome additions to the food analysis toolkit.

References

  1. Schmidt, A. and Strube, J. (2018). Application and Fundamentals of Liquid-Liquid Extraction Processes: Purification of Biologicals, Botanicals, and Strategic Metals. In John Wiley & Sons, Inc (Ed.), Kirk-Othmer Encyclopedia of Chemical Technology. (pp. 1–52).
  2. Musteata, M. and Musteata, F. (2011). Overview of extraction methods for analysis of vitamin D and its metabolites in biological samples. Bioanalysis, 3(17), 1987–2002.

 

FDA

More Cases of Cyclospora Reported from Bagged Salads, Pathogen Found in Irrigation Canal

By Food Safety Tech Staff
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FDA

Learn more about food safety supply chain management & traceability during the 2020 Food Safety Consortium Virtual Conference SeriesThe FDA and CDC have been investigating a multistate outbreak of Cyclospora involving bagged salads from Fresh Express since June. Although the products were recalled and should no longer be available in retail locations, the CDC continues to report more cases. As of August 12, 2020, the CDC counted 690 people with laboratory-confirmed Cyclospora infections throughout 13 states. Thirty-seven people have been hospitalized, and no deaths have been reported.

As the FDA conducted its traceback investigation to find the source of the outbreak linked to the Fresh Express products, the agency was able to identify several farms. It analyzed water samples from two public access points along a regional water management canal (C-23) west of Port St. Lucie, Florida. Using the FDA’s validated testing method, the samples tested positive for Cyclospora cayetanensis. However, it is important to note that the Cyclospora found might not be a direct match to the pathogen found in the clinical cases.

According to FDA: “Given the emerging nature of genetic typing methodologies for this parasite, the FDA has been unable to determine if the Cyclospora detected in the canal is a genetic match to the clinical cases, therefore, there is currently not enough evidence to conclusively determine the cause of this outbreak. Nevertheless, the current state of the investigation helps advance what we know about Cyclospora and offers important clues to inform future preventive measures.”

The agency’s traceback investigation is complete, but the cause or source of the outbreak has not been determined. The investigation also revealed that carrots are no longer of interest at as part of the outbreak, but red cabbage and iceberg lettuce are still being investigated. FDA is also working with Florida and the area’s local water district to learn more about the source of Cyclospora in the canal.

Karen Everstine, Decernis
Food Fraud Quick Bites

Adulteration of Botanical Ingredients

By Karen Everstine, Ph.D.
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Karen Everstine, Decernis

Botanical ingredients are important to the food and beverage industries as well as the dietary supplements industry. Botanicals are plants or specific plant parts (leaves, roots, bark, berries, etc.) that are used for particular properties. These properties can be therapeutic or related to color, flavor or other attributes. Botanicals include extracts such as Ginkgo biloba, saw palmetto, and elderberry as well as herbs and spices used in cooking, essential oils, pomegranate juice and extracts, and olive oil. There is a substantial overlap between botanical products used in the herb and supplement industries and those used in foods and beverages. Many “conventional” foods and beverages include botanical extracts or other ingredients to advertise a therapeutic effect.

In 2014, FDA issued a final guidance for industry related to labeling of liquid dietary supplements (vs. beverages). FDA noted, in their rationale for the guidance, two trends:

“First, we have seen an increase in the marketing of beverages as dietary supplements, in spite of the fact that the packaging and labeling of many liquid products represent the products as conventional foods. Products that are represented as conventional foods do not meet the statutory definition of a dietary supplement…and must meet the regulatory requirements that apply to conventional foods.

Second, FDA has seen a growth in the marketplace of beverages and other conventional foods that contain novel ingredients, such as added botanical ingredients or their extracts. Some of these ingredients have not previously been used in conventional foods and may be unapproved food additives. In addition, ingredients that have been present in the food supply for many years are now being added to beverages and other conventional foods at levels in excess of their traditional use levels or in new beverages or other conventional foods. This trend raises questions regarding whether these ingredients are unapproved food additives when used at higher levels or under other new conditions of use. Some foods with novel ingredients also bear claims that misbrand the product or otherwise violate the FFDCA.”

The American Botanical Council (ABC) has been publishing information on the safe, responsible and effective use of botanicals since 1988, including the quarterly journal HerbalGram and a book of herb monographs The ABC Clinical Guide to Herbs. In order to help combat the increasing problem of adulteration in the industry, the Botanical Adulterants Prevention Program (BAPP) was launched in 2010 by ABC along with the American Herbal Pharmacopeia and the University of Mississippi National Center for Natural Products Research. The goal of BAPP is to educate members of the herbal and dietary supplement industry about ingredient and product adulteration through the publication of documents such as adulteration bulletins and laboratory guidance documents. The information in these documents helps ensure the identity, authenticity and safety of botanicals along the supply chain.

Karen Everstine will be discussing food fraud during the 2020 Food Safety Consortium Virtual Conference Series | An example of the Botanical Adulterants Prevention Bulletin for cranberry is seen in Figure 1. It includes a description of the species that can be labeled as cranberry in the United States, a brief description of the marketplace, information on potential adulterants in cranberry fruit extract and other cranberry products, and guidance on analytical methods to test cranberry products for adulteration.

Cranberry adulteration, Botanical Adulterants Bulletin
Figure 1 courtesy of Decernis and the Botanical Adulterants Bulletin.

Decernis has been working with the Botanical Adulterants Prevention Program (BAPP) to integrate links to their expert content into the Food Fraud Database (FFD). This will ensure our users can better develop ingredient specifications, manage risk, and protect their consumers by leveraging this content for food fraud and herbal ingredient fraud prevention. We are currently incorporating three types of BAPP documents into FFD:

  • Adulterants Bulletins. Information and links to these documents will be entered as Inference records in FFD. We are extracting ingredient and adulterant names (including Latin names as synonyms) from the document, assigning “Reasons for Adulteration,” and providing a link to the full document on the BAPP website.
  • Adulteration Reports. Information and links to these documents will also be entered as Inference records in FFD. We are extracting ingredient and adulterant names from the document, assigning “Reasons for Adulteration,” and providing a link to the full document on the BAPP website.
  • Laboratory Guidance documents. Information and links to these documents will be entered as both method record and inference records in FFD. We are extracting ingredient and adulterant names from the document, assigning “Reasons for Adulteration,” and providing a link to the full document on the BAPP website.

Decernis analysts are currently integrating this content into FFD, which will be uploaded to the system between now and early September.

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Olive Oil, Again And Again

By Susanne Kuehne
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Susanne Kuehne, Decernis
Olive Oil
Find records of fraud such as those discussed in this column and more in the Food Fraud Database.
Image credit: Susanne Kuehne.

Fraudulent olive oil made its way into the retail market in Brazil. More than 1300 bottles of product labeled extra virgin olive oil were seized, the oil was analyzed and found to be fraudulent. An investigation about the source of the adulteration and whether the fraud happened at the producer or in retail is still ongoing.

Resource

  1. Samara, O. and Ferreira, C. (June 2, 2020) “Equipe da Decon apreende mais de 1.300 frascos de azeite adulterados na Grande Vitória”. Polícia Civil do Espírito Santo (PCES).
Are Traasdahl, Crisp
FST Soapbox

How a History of Slow Technology Adoption Across Food Supply Chains Nearly Broke Us

By Are Traasdahl
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Are Traasdahl, Crisp

The COVID-19 crisis has exacerbated existing disconnects between food supply and demand. While some may be noticing these issues on a broader scale for the first time, the reality is that there have been challenges in our food supply chains for decades. A lack of accurate data and information sharing is the core of the problem and had greater impact due to the pandemic. Outdated technologies are preventing advancements and efficiencies, resulting in the paradox of mounting food insecurity and food waste.

To bridge this disconnect, the food industry needs to implement innovative AI and machine learning technologies to prevent shortages, overages and waste as COVID-19 subsides. Solutions that enable data sharing and collaboration are essential to build more resilient food supply chains for the future.

Data-sharing technologies that can help alleviate these problems have been under development for decades, but food supply chains have been slow to innovate compared to other industries. By reviewing the top four data-sharing technologies used in food industry and the year they were introduced to food supply chains, it’s evident that the pace of technology innovation and adoption needs to accelerate to advance the industry.

A History of Technology Adoption in the Food Industry

The Barcode – 19741
We’re all familiar with the barcode—that assemblage of lines translated into numbers and letters conveying information about a product. When a cashier scans a barcode, the correct price pops up on the POS, and the sale data is recorded for inventory management. Barcodes are inexpensive and easy to implement. However, they only provide basic information, such as a product’s name, type, and price. Also, while you can glean information from a barcode, you can’t change it or add information to it. In addition, barcodes only group products by category—as opposed to radio-frequency identification (RFID), which provides a different code for every single item.

EDI First Multi-Industry Standards – 19812
Electronic data interchange (EDI) is just what it sounds like—the concept of sharing information electronically instead of on paper. Since EDI standardizes documents and the way they’re transferred, communication between business partners along the supply chain is easier, more efficient, and human error is reduced. To share information via EDI, however, software is required. This software can be challenging for businesses to implement and requires IT expertise to handle updates and maintenance.

RFID in the Food Supply Chain – 20033
RFID and RFID tags are encoded with information that can be transmitted to a reader device via radio waves, allowing businesses to identify and track products and assets. The reader device translates the radio waves into usable data, which then lands in a database for tracking and analysis.

RFID tags hold a lot more data than barcodes—and data is accessible in remote locations and easily shared along the supply chain to boost transparency and trust. Unlike barcode scanners, which need a direct line of sight to a code, RFID readers can read multiple tags at once from any direction. Businesses can use RFID to track products from producer to supplier to retailer in real time.

In 2003, Walmart rolled out a pilot program requiring 100 of its suppliers to use RFID technology by 2005.3 However, the retail giant wasn’t able to scale up the program. While prices have dropped from 35–40 cents during Walmart’s pilot to just 5 cents each as of 2018, RFID tags are still more expensive than barcodes.4 They can also be harder to implement and configure. Since active tags have such a long reach, businesses also need to ensure that scammers can’t intercept sensitive data.

Blockchain – 20175
A blockchain is a digital ledger of blocks (records) used to record data across multiple transactions. Changes are recorded in real-time, making the history unfalsifiable and transparent. Along the food supply chain, users can tag food, materials, compliance certificates and more with a set of information that’s recorded on the blockchain. Partners can easily follow the item through the physical supply chain, and new information is recorded in real-time.

Blockchain is more secure and transparent, less vulnerable to fraud, and more scalable than technologies like RFID. When paired with embedded sensors and RFID tags, the tech offers easier record-keeping and better provenance tracking, so it can address and help solve traceability problems. Blockchain boosts trust by reducing food falsification and decreasing delays in the supply chain.6

On the negative side, the cost of transaction processing with blockchain is high. Not to mention, the technology is confusing to many, which hinders adoption. Finally, while more transparency is good news, there’s such a thing as too much transparency; there needs to be a balance, so competitors don’t have too much access to sensitive data.

Cloud-Based Demand Forecasting – 2019 to present7
Cloud-based demand forecasting uses machine learning and AI to predict demand for various products at different points in the food supply chain. This technology leverages other technologies on this list to enhance communication across supply chain partners and improve the accuracy of demand forecasting, resulting in less waste and more profit for the food industry. It enables huge volumes of data to be used to predict demand, including past buying patterns, market changes, weather, events and holidays, social media input and more to create a more accurate picture of demand.

The alternative to cloud-based demand forecasting that is still in use today involves Excel or manual spreadsheets and lots of number crunching, which are time-intensive and prone to human error. This manual approach is not a sustainable process, but AI, machine learning and automation can step in to resolve these issues.

Obtaining real-time insights from a centralized, accurate and accessible data source enables food suppliers, brokers, distributors, brands and retailers to share information and be nimble, improving their ability to adjust supply in response to factors influencing demand.8 This, in turn, reduces cost, time and food waste, since brands can accurately predict how much to produce down to the individual SKU level, where to send it and even what factors might impact it along the way.

Speeding Up Adoption

As illustrated in Figure 1, the pace of technology change in the food industry has been slow compared to other industries, such as music and telecommunications. But we now have the tools, the data and the brainpower to create more resilient food supply chains.

Technology adoption, food industry
Figure 1. The pace of technology change in the food industry has been slow compared to other industries. Figure courtesy of Crisp.

Given the inherent connectivity of partners in the food supply chain, we now need to work together to connect information systems in ways that give us the insights needed to deliver exactly the rights foods to the right places, at the right time. This will not only improve consumer satisfaction but will also protect revenue and margins up and down food supply chains and reduce global waste.

References

  1. Weightman, G. (2015). The History of the Bar Code. Smithsonian Magazine.
  2. Locken, S. (2012). History of EDI Technology. EDI Alliance.
  3. Markoff, R, Seifert, R. (2019). RFID: Yesterday’s blockchain. International Institute for Management Development.
  4. Wollenhaupt, G. (2018). What’s next for RFID? Supply Chain Dive.
  5. Tran, S. (2019). IBM Food Trust: Cutting Through the Complexity of the World’s Food Supply with Blockchain. Blockchain News.
  6. Galvez, J, Mejuto, J.C., Simal-Gandara, J. (2018). Future Challenge on the use of blockchain for food traceability analysis. Science Direct.
  7. (2019). Crisp launches with $14.2 million to cut food waste using big data. Venture Beat.
  8. Dixie, G. (2005). The Impact of Supply and Demand. Marketing Extension Guide.
Susanne Kuehne, Decernis
Food Fraud Quick Bites

Now It’s Easier To Bee Happy

By Susanne Kuehne
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Susanne Kuehne, Decernis
Food fraud, honey, sunflower
Find records of fraud such as those discussed in this column and more in the Food Fraud Database. Image credit: Susanne Kuehne

Honey is an easy target for food fraud and adulteration with sucrose, high fructose corn syrup, molasses and other sugars are not uncommon. To quickly identify adulterants, a method using Raman spectroscopy and pattern recognition analysis was developed. To verify the method, 97 samples were tested with the new method, and the tests confirmed with HPLC, with the result that 17% of the commercial honey samples showed fraud from added sugars.

Resource

  1. Aykas, D.P., et al. (May 5, 2020). “Authentication of commercial honeys based on Raman fingerprinting and pattern recognition analysis”. Science Direct.

 

RS Spectra

Using Raman Spectroscopy to Evaluate Packaging for Frozen Hamburgers

By Gary Johnson, Ph.D.
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RS Spectra

Raman spectroscopy (RS) can be used to identify layers in polymer food packaging films to better understand the laminated plastic’s chemical composition. A Raman spectrum is obtained by illuminating a sample with a laser and collecting and measuring scattered light with a spectrometer. Coupling the spectrometer to a microscope with a mapping stage allows an accurate way to create a chemical map of a film’s composition and structure. The map provides valuable information to better understand the packaging’s barrier properties, structural integrity and layers.

The RS method can be useful for conducting failure analysis (why did a food package fail to meet standards), supply chain validation (is the plastic what the supplier claims), decision making (which plastic should be used), and evaluating package appearance (why is there discoloring, haze or particle inclusions in the film). It provides important information for design, purchasing, product success and other decisions that food manufacturers and packagers regularly face.

Take for example the packaging used for frozen hamburger patties. The film used must be transparent to display the hamburger patties, but it also needs to provide an oxygen barrier in order to prevent the ground beef from turning brown. As such, a polymer layer with low oxygen permeability must be incorporated into the laminated film, along with other components like nylon for strength and polyethylene for heat sealing and water barrier. The most common polymer used as an oxygen barrier is ethylene-vinyl alcohol copolymer (EVOH).

It is important that the film used to package these hamburger patties includes a good heat seal as well as a proper oxygen barrier layer. The possible absence of either of these could result in the undesired effect of ground beef turning brown. Manufacturers may want to test packaging for an EVOH layer to make a purchasing decision or verify a supplier’s claims. Additionally, if the packaging fails, an analysis can determine if the failure was due to having no EVOH barrier layer in the product or if there is a need to investigate other potential issues with the packaging. Regardless of the reason, RS provides a preferable method for rapidly evaluating the plastic for an EVOH oxygen barrier layer.

The RS method can be used to determine the construction of the laminated film and confirm that it meets specifications. Using the combination of RS with microscopy and mapping allows both identification of the polymers and the evaluator to correlate the composition to the layer structure of the laminated film. This method provides a map showing the composition of each layer in the film. In some cases, the Raman map will show layers that are not resolved in the visible micrograph image. Thus, with RS, one test provides both the structure and composition of each layer of the laminated film.

Laminated film, packaging, Intertek
This sample table illustrates composition and thickness of each layer of a laminated film. Table courtesy of Intertek.

To start, a small section of the film (5 x 10 mm) is cut and mounted with a photocuring resin. A cross section of the mounted film is then cut to expose the layers for analysis. This cross-section is placed on the mapping microscope stage of the Raman instrument. A micrograph image with a 100X objective is obtained and a Raman map of the cross-section with 1 µm2 pixel resolution collected.

A map image is obtained by classical least squares (CLS) fitting example spectra to each of the spectra collected from the cross-section. The example spectra for the CLS fits are averages (mean) of the spectra in the center of each layer with a unique composition as determined by the data (see Figure 1). The final result is a color-coded map that can be superimposed on the micrograph image to show the composition and thickness of each layer in the laminated film. For example, a film with six layers composed of Nylon 6, polyethylene or EVOH would have varying thickness and placement of each layer to achieve the desired result for the product.

RS Spectra
Figure 1. Example spectra used to create the CLS model for map image.

The composition map can confirm the presence of an oxygen barrier layer of EVOH, as well as the overall construction of the laminated film. Knowing the thickness of the barrier layer is important since the gas permeability is a function of the film thickness. Determination of the overall film structure allows the end-user to confirm the film meets the specifications from the supplier. In turn, this can be used to make important purchasing decisions or insights into what caused a packaging failure.

While good, successful results will confirm the presence of an EVOH layer, the RS map may also show only polymers that don’t have the required oxygen barrier properties (see Figure 2). The manufacturer would need to check it against a supplier spec sheet. It may ultimately show that the lack of an EVOH layer is what caused the issue with the packaging. If the test is being used for decision-making purposes, the manufacturer would know not to use the product. If a supply chain validation is being run, after checking the spec sheet, the manufacturer may need to correct the situation.

Raman spectroscopy
Figure 2. Raman map overlaid with image of film cross section. Green = nylon; Red = polyethylene; Yellow = ethylene vinyl alcohol copolymer (EVOH).

What if the analysis confirmed that an EVOH layer was present, but the test was done for a failure analysis, meaning the packaging did fail at some point? If the EVOH later is present but the meat is still turning brown and/or spoiling, other potential problems would need to be evaluated. In this case, the issues would most likely be with the heat seal and additional testing of the heat seal would be necessary. Thanks to the RS analysis, the investigation into the packaging failure can proceed, and the issue with the heat seal identified.

By giving a chemical image of the packaging, RS analysis provides a wealth of information about a film that can be vital to a food manufacturer or processor. Knowing why certain films may not be working, either due to faults in chemical makeup or the need to look elsewhere, such as the heat seal, RS quickly and efficiently provides information and answers to help get products to market and meet consumer demand.

Chocolate

Chocolate and Big Data: The Recipe for Food Safety Is Changing

By Steven Sklare
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Chocolate

Almost everybody loves chocolate, an ancient, basic, almost universal and primal source of pleasure. “The story of chocolate beings with cocoa trees that grew wild in the tropical rainforests of the Amazon basin and other areas in Central and South America for thousands of years… Christopher Columbus is said to have brought the first cocoa beans back to Europe from his fourth visit to the New World” between 1502 and 1504.1

Unfortunately, the production of chocolate and chocolate products today is as complex as any other global food product with supply chains that reach from one end of the world to the other. The complexity of the supply chain and production, along with the universal demand for the finished product, exposes chocolate to increasing pressure from numerous hazards, both unintentional and intentional. For example, we know that more than 70% of cocoa production takes place in West African countries, particularly the Ivory Coast and Ghana. These regions are politically unstable, and production is frequently disrupted by fighting. While production has started to expand into more stable regions, it has not yet become diversified enough to normalize the supply. About 17% of production takes place in the Americas (primarily South America) and 9% from Asia and Oceania.2

In today’s world of global commerce these pressures are not unique to chocolate. Food quality and safety experts should be armed with tools and innovations that can help them examine specific hazards and fraud pertaining to chocolate and chocolate products. In fact, the global nature of the chocolate market, requires fast reflexes that protect brand integrity and dynamic quality processes supported by informed decisions. Digital tools have become a necessity when a fast interpretation of dynamic data is needed. If a food organization is going to effectively protect the public’s health, protect their brand and comply with various governmental regulations and non-governmental standards such as GFSI, horizon scanning, along with the use of food safety intelligent digital tools, needs to be incorporated into food company’s core FSQA program.

This article pulls information from a recent industry report about chocolate products that presents an examination of the specific hazards and fraud pertaining to chocolate and chocolate products along with ways to utilize this information.

Cocoa and chocolate products rely on high quality ingredients and raw materials, strict supplier partnership schemes and conformity to clearly defined quality and safety standards. During the past 10 years there have been a significant number of food safety incidents associated with chocolate products. The presence of Salmonella enterica, Listeria monocytogenes, allergens and foreign materials in cocoa/chocolate products have been reported on a global scale. Today, information on food safety incidents and potential risks is quickly and widely available by way of the internet. However, because the pertinent data is frequently siloed, food safety professionals are unable to take full advantage of it.

Top Emerging Hazards: Chocolate Products (2013-2018)

Publicly available data, from sources such as European Union RASFF, Australian Competition and Consumer Commission, UK Food Standards Agency, FDA, Food Standards Australia New Zealand (FSANZ), shows a significant increase in identified food safety incidents for cocoa/chocolate products from 2013 to 2018. For this same time period, the top emerging hazards that were identified for chocolate products were the following:

  • Allergens: 51.60%
  • Biological: 16.49%
  • Foreign bodies: 13.83%
  • Chemical: 7.45%
  • Fraud: 6.38%
  • Food additives & flavorings: 4.26%
  • Other hazards: 2.66%

By using such information to identify critical food safety protection trends, which we define to include food safety (unintentional adulteration) and food fraud (intentional adulteration, inclusive of authenticity/intentional misrepresentation) we can better construct our food protection systems to focus on the areas that present the greatest threats to public health, brand protection and compliance.

A Data Driven Approach

Monitoring Incoming Raw Materials
Assessment and identification of potential food protection issues, including food safety and fraud, at the stage of incoming raw materials is of vital importance for food manufacturers. Knowledge of the associated risks and vulnerabilities allows for timely actions and appropriate measures that may ultimately prevent an incident from occurring.

Specifically, the efficient utilization of global food safety and fraud information should allow for:

  • Identification of prevalent, increasing and/or emerging risks and vulnerabilities associated with raw materials
  • Comparative evaluation of the risk profile for different raw materials’ origins
  • Critical evaluation and risk-based selection of raw materials’ suppliers

A comprehensive risk assessment must start with the consideration of the identified food safety incidents of the raw material, which include the inherent characteristics of the raw material. Next, the origin-related risks must be taken into account and then the supplier-related risks must be examined. The full risk assessment is driven by the appropriate food safety data, its analysis and application of risk assessment scientific models on top of the data.

Using food safety intelligent digital tools to analyze almost 400 unique, chocolate product related food safety incidents around the globe provides us with important, useful insights about cocoa as a raw material, as a raw material from a specific origin and as a raw material being provided by specific suppliers. The graph below represents the results of the analysis illustrating the trend of incidents reported between 2002 and 2018. It can be observed that after a significant rise between 2009 and 2010, the number of incidents approximately doubled and remained at that level for the rest of the evaluated period (i.e., from 2010 to 2018), compared to the period from 2002 to 2005.

Cocoa incidents, FOODAKAI
Graph from Case Study: Chocolate Products: lessons learned from global food safety and fraud data and the guidance it can provide to the food industry,
an industry report from FOODAKAI. Used with permission.

By further analyzing the data stemming from the 400 food safety incidents and breaking them down into more defined hazards, for incoming raw materials, we can clearly see that chemical hazards represent the major hazard category for cocoa.

  • Chemical: 73.46%
  • Biological: 16.49%
  • Organoleptic aspects: 5.93%
  • Other Hazards: 4.38%
  • Fraud: 2.32%
  • Foreign bodies: 2.06%
  • Food additives and flavorings: .77%
  • Allergens: .52%
  • Food contact materials: .52%

Using the appropriate analytical tools, someone can drill down into the data and identify the specific incidents within the different hazard categories. For example, within the “chemical hazard” category specific hazards such as organophosphates, neonicotinoids, pyrethroids and organochlorines were identified.

Comparative Evaluation of Risk Profiles for Different Origins of Raw Materials
The main regions of origin for cocoa globally are Africa, Asia and South America. After collecting and analyzing all relevant data from recalls and border rejections and the frequency of pertinent incidents, we can accurately identify the top hazards for cocoa by region.

The top five specific hazards for the regions under discussion are listed in Table I.

Africa South America Asia
1 Organophosphate 2,4-dinitrophenol (DNP) 2,4-dinitrophenol (DNP)
2 Molds Pyrethroid Poor or insufficient controls
3 Neonicotinoid Aflatoxin Aflatoxin
4 Pyrethroid Cadmium Spoilage
5 Organochlorine Anilinopyrimidine Salmonella
Table I.  Top Five Hazards By Region

After the first level of analysis, a further interpretation of the data using the appropriate data intelligence tools can help to reach to very specific information on the nature of the incidents. This provides additional detail that is helpful in understanding how the regional risk profiles compare. For example, the prevalence of chemical contamination, as either industrial contaminants or pesticides, has been a commonly observed pattern for all three of the regions in Table I. However, beyond the general hazard category level, there are also different trends with regard to specific hazards for the three different regions. One such example is the increased presence of mold in cocoa beans coming from Africa.

The primary hazard categories for cocoa, as a raw ingredient were identified and a comparison among the primary hazards for cocoa by region (origin-specific) should take place. The next step in a data-powered supplier assessment workflow would be to incorporate our use of global food safety data in evaluating the suppliers of the raw materials.

The Role of Global Food Safety Data

This article has been focused on chocolate products but has only touched the surface in terms of the information available in the complete report, which also includes specific information about key raw materials. Let’s also be clear, that the techniques and tools used to generate this information are applicable to all food products and ingredients. As we strive to produce food safely in the 21st Century and beyond, we must adapt our methods or be left behind.

The regulatory environment the food industry must operate in has never been more intense. The threats to an organization’s brand have never been greater. This is not going to change. What must change is the way in which food companies confront these challenges.

Global food safety data can contribute to the establishment of an adaptive food safety/QA process that will provide time savings and improve a quality team’s efficiency and performance.

Based on the continuous analysis of food recalls and rejections by key national and international food authorities, a food safety / quality assurance manager could establish an adaptive supplier verification process and risk assessment process by utilizing the knowledge provided by such data. In that way, QA, procurement, food safety and quality departments can be empowered with critical supplier data that will inform the internal procedures for incoming materials and ingredients (e.g., raw materials, packaging materials) and allow for adaptive laboratory testing routines and compliance protocols. Moreover, food safety systems can become adaptive, enabling quality assurance and safety professionals to quickly update points of critical control when needed, and intervene in important stages of the chocolate manufacturing process.

References

  1. Discovering Chocolate. The Great Chocolate Discovery. Cadbury website. Retrieved from https://www.cadbury.com.au/About-Chocolate/Discovering-Chocolate.aspx.
  2. Chocolate Industry Analysis 2020 – Cost & Trends. Retrieved from https://www.franchisehelp.com/industry-reports/chocolate-industry-analysis-2020-cost-trends/.