Tag Archives: Testing

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.

 

Susanne Kuehne, Decernis
Food Fraud Quick Bites

A New Way Of Greenwashing

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

Turkish delight, baklava, halva, biscotti, mortadella, ice cream and many more delicious foods from around the world contain pistachios, which are pricey and therefore a popular target for food fraud. A recent article describes a method to detect spinach and green peas that often are used as a pistachio replacement due to their color and low price. The technique combines NIR (near infrared) spectroscopy and chemometric analysis and provides a method that is precise, fast and non-destructive.

Resource

  1. Genis, H.E., et al. (August 15, 2020). “Determination of green pea and spinach adulteration in pistachio nuts using NIR spectroscopy”. Science Direct. LWT.
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).
Alex Kinne, Thermo Fisher Scientific
In the Food Lab

Ensuring Food Safety in Meat Processing Through Foreign Object Detection

By Alex Kinne
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Alex Kinne, Thermo Fisher Scientific

The USDA estimates that foodborne illnesses cost more than $15.6 billion each year. However, biological contamination isn’t the only risk to the safety and quality of food. Food safety can also be compromised by foreign objects at virtually any stage in the production process, from contaminants in raw materials to metal shavings from the wear of equipment on the line, and even from human error. While the risk of foreign object contamination may seem easy to avoid, in 2019 alone the USDA reported 34 food recalls, impacting 17 million pounds of food due to ‘extraneous material’ which can include metal, plastic and even glass.

When FSMA went into effect, the focus shifted to preventing food safety problems, necessitating that food processors implement preventive controls to shift the focus from recovery and quarantine to proactive risk mitigation. Food producers developed Hazard Analysis and Critical Control Point (HACCP) plans focused on identifying potential areas of risk and placement of appropriate inspection equipment at these key locations within the processing line.

Metal detection is the most common detection technology used to find ferrous, non-ferrous, and stainless steel foreign objects in food. In order to increase levels of food safety and better protect brand reputation, food processors need detection technologies that can find increasingly smaller metal foreign objects. Leading retailers are echoing that need and more often stipulate specific detection performance in their codes of practice, which processors must meet in order to sell them product.

As food processors face increased consumer demand and continued price-per-unit pressures, they must meet the challenges of greater throughput demands while concurrently driving out waste to ensure maximum operational efficiencies.

Challenges Inherent in Meat Metal Detection

While some food products are easier to inspect, such as dry, inert products like pasta or grains, metal foreign object detection in meat is particularly challenging. This is due to the high moisture and salt content common in ready-to-eat, frozen and processed, often spicy, meat products that have high “product effect.” Bloody whole muscle cuts can also create high product effect.

The conductive properties of meat can mimic a foreign object and cause metal detectors to incorrectly signal the presence of a physical contaminant even when it is nonexistent. Food metal detectors must be intelligent enough to ignore these signals and recognize them as product effect to avoid false rejection. Otherwise, they can signal metal when it is not present, thus rejecting good product and thereby increasing costs through scrap or re-work.

Equipping for Success

When evaluating metal detection technologies, food processors should request a product test, which allows the processor to see how various options perform for their application. The gold standard is for the food processor to send in samples of their product and provide information about the processing environment so that the companies under consideration can as closely as possible simulate the manufacturing environment. These tests are typically provided at no charge, but care should be taken upfront to fully understand the comprehensiveness of the testing methodologies and reporting.

Among the options to explore are new technologies such as multiscan metal detection, which enables meat processors to achieve a new level of food safety and quality. This technology utilizes five user-adjustable frequencies at once, essentially doing the work of five metal detectors back-to-back in the production line and yielding the highest probability of detecting metal foreign objects in food. When running, multiscan technology allows inspectors to view all the selected frequencies in real time and pull up a report of the last 20 rejects to see what caused them, allowing them to quickly make appropriate adjustments to the production line.

Such innovations are designed for ease of use and to meet even the most rigorous retailer codes of practice. Brands, their retail and wholesale customers, and consumers all benefit from carefully considered, application-specific, food safety inspection.

Ensuring Safety

The food processing industry is necessarily highly regulated. Implementing the right food safety program needs to be a top priority to ensure consumer safety and brand protection. Innovative new approaches address these safety concerns for regulatory requirements and at the same time are designed to support increased productivity and operational efficiency.

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Le Bordeaux, C’est Si Beau!

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

This kind of lead must weigh heavily on the minds of food and beverage fraudsters. The quantity of lead isotopes and elemental lead can be used to determine the geographic origin and vintage of a wine and therefore determine whether the wine is from a specific location. The isotopic profiles of genuine Bordeaux wines were compared to suspicious bottling. The fake wines were clearly identified to be from different locations and vintages than claimed on the labels.

Resources

  1. Taylor, P. (September 16, 2019). “Lab technique spots fake Bordeaux wines”. Securing Industry.
  2. Epova, E. (January 15, 2020). “Potential of lead elemental and isotopic signatures for authenticity and geographical origin of Bordeaux wines”. Food Chemistry.

 

Coronavirus, COVID-19

China Stops Poultry Imports From Tyson Foods Due to COVID-19 Concerns, Clamping Down on Inspections

By Food Safety Tech Staff
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Coronavirus, COVID-19

On Sunday China’s General Administration of Customs announced that it would be suspending imported shipments of poultry from a Tyson Foods plant based in Springdale, Arkansas. The suspension is reportedly due to an outbreak of coronavirus cases at the facility.

On Friday Tyson Foods announced the results of COVID-19 testing conducted at its facilities in northwestern Arkansas (Benton and Washington counties): 3,748 employees were tested; 481 tested positive, and 95% were asymptomatic.

“The results across our Northwest Arkansas facilities, and the country more broadly, reflect how much is still unknown about this virus, which is why Tyson is committed to providing information to our local health officials and enhanced education to our team members,” said Tom Brower, senior vice president of health and safety for Tyson Foods stated in a company press release. “Through our inclusive approach to large-scale testing, we are finding that a very high level of team members who test positive do not show symptoms. Identifying asymptomatic cases helps the community, since other testing is often limited to people who feel unwell.”

Meanwhile, it has also been reported that officials in China want the inspection process of overseas shipments ramped up, as they suspect that COVID-19 could be present on imported frozen food products.

Over the weekend PepsiCo’s Beijing operations were suspended following confirmed coronavirus cases at its chips production facility.

Last week new cases of the coronavirus were reported in Beijing, leading to concerns of a resurgence of the virus. Some new cases have been linked to the Xinfadi Market, a wholesale food market.

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Milking The Business

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

Milk has enjoyed increasing popularity in China, however, the milk supply chain is still vulnerable to fraud throughout the country. Milk can be adulterated in variety of ways, from dilution with water to the addition of carbohydrate- or nitrogen-based and protein-rich adulterants as well as a variety of unapproved (sometimes hazardous) additives. This study used Fourier transform-infrared spectroscopy to determine fraud in 52 ultra-high-temperature commercial milk samples. Twenty-three percent of the samples turned out to be adulterated and some of the samples were even flagged for multiple issues.

Resource

  1. Yuzheng Y., et.al. (June 1, 2020) “Prevalence of Milk Fraud in the Chinese Market and its Relationship with Fraud Vulnerabilities in the Chain.” MDPI.