Tag Archives: product integrity

John Silliker

Mérieux NutriSciences Honors Founder with Silliker Food Science Center

By Food Safety Tech Staff
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John Silliker

Mérieux NutriSciences, which offers analytical and product development solutions to prevent health risks related to the food, beverage and nutraceutical industries, has renamed its food research center the Silliker Food Science Center in honor of the company’s founder, Dr. John H. Silliker.

When Dr. Silliker founded his first laboratory in 1967, he became a leading figure in the fight against Salmonella and for food safety. He used science to develop practical and innovative solutions to answer food industry challenges. His work—as well as his philosophy of inspire, discover and innovate—continues to guide Mérieux NutriSciences’s approach as the company celebrates its 55th anniversary.

The company shared that the Silliker Food Science Center will continue Dr. Silliker’s mission by embracing his core philosophy to:

Inspire: Dr. Silliker has inspired generations of scientists. It’s with this inspiration that the center’s team stands ready to continue the tradition of developing science and lead contract research projects for the food industry.

Discover: Dr. Silliker’s fundamental principle was to provide a place to go when you need to know. This drive the center’s scientists to work alongside food companies to solve their unique challenges with shelf life extension, product integrity and method applicability.

Innovate: Dr. Silliker continually pushed the boundaries of innovation which is continued today by the scientists at the Silliker Food Science Center, which helps to:

  • Conduct critical investigations and root cause analysis through advanced technologies
  • Understand product defect
  • Validate food manufacturing process
  • Support product development and improve product shelf life
  • Ensure matrix is fit for analytical method


In-line micro-hole detection

Technologies for In-line Monitoring of Micro-Holes in Packaging

By Paolo Tondello
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In-line micro-hole detection

In-line verification for the presence of micro-holes throughout food packaging production is possible by means of an innovative application of IR (Infrared) spectroscopy, or via gas sensors capable of detecting the leakage of target molecules present inside packages.

The areas of application sectors can be modified atmosphere packaging (MAP) packaged products, bakery products preserved with alcohol, food products preserved in nitrogen or air whose release of aromas can be detected.

Today, there are many preservation technologies available on the market for packaged food that lengthen the product’s shelf life while ensuring its organoleptic characteristics and food safety. Replacing air with a gas mixture (MAP) or with nitrogen, or by adding alcohol, are some preservation methods that cover a wide range of products. For all products, it is essential to check:

  • The type of packaging, correctly barrier-coated to prevent the leakage of any preservation substances
  • The gas mixture for MAP packaged products is correct for the type of product
  • The presence of alcohol inside the package for bakery products
  • Via seal test

This last point, checking for the presence of micro-holes in the packaging, is crucial to avoid thwarting all efforts to optimize the packaging’s preservation mixture. Therefore, let’s examine how it is possible to perform a seal test, and the innovations brought about by IR spectroscopy technology that introduce important elements of in-line monitoring of the presence of micro-holes in packaging and the seal’s integrity.

In-line micro-hole detection
Checking for the presence of micro-holes in the packaging, is crucial to avoid thwarting all efforts to optimize the packaging’s preservation mixture. Image courtesy of FT System.

Micro-Holes in Packaging: Consequences of Spot Checks

The presence of a micro-hole in packaging is a particularly critical problem in the food industry, since it can lead to poor food preservation and the loss of its organoleptic characteristics—as well as the possible formation of mold.

Micro-holes may form as a result of defective sealing processes or during the various processing stages of the package, and can lead to negative consequences of the product days later, when the package is already in the shop or on the shelf of a supermarket. Therefore, it is important to make sure the container is intact during the production stage.

The procedures normally in use today to check for micro-holes are spot checks, which detect the loss of pressure or leakage of gas from the package by immersing the product in water, or via an instrument that applies a “dry” vacuum. In the first case, which is called a bubble test, the product is immersed in a container filled with water that is hermetically sealed and to which an external vacuum is applied. This encourages bubbles to come out from any micro-holes, which can, at this point, be checked visually or by means of a camera.

In the second case, a vacuum is created that is carried out by placing the package inside a bell. The molecules leaked from the package (such as CO2 in the case of MAP products) or loss of pressure are indications of the presence of a micro-hole.

The main limitation of these methods is, first and foremost, that of being destructive, since it is no longer possible to reuse the tested package. Over and above this is the fact that they are, of course, merely spot checks—and therefore not comprehensive in their analysis.

Spot-checking does not check the integrity of the entire production, which means that defects are not detected on a regular basis. Moreover, this method is costly in terms of re-processing batches should a micro-hole be detected in the batch being tested.

Modern Applications for Testing In-Line Micro-Holes

The need for in-line identification of micro-holes on 100% of production is pressing, and research for possible solutions has been focused on this need in recent years. Technology is needed that must be:

  • Rapid, in order to be applied to the line’s speed;
  • Reliable in detecting micro-holes;
  • With few false rejects, even at high speed;
  • Characterized by low maintenance costs;
  • Easily manageable for format changes, which are becoming increasingly frequent in production.

This has all been made possible by means of application of IR spectroscopy, or the use of gas sensors for in-line inspection of the presence of holes and micro-holes. These non-destructive technologies make it possible to detect in-line leakages in packaging, package by package, by identifying target escaping molecules.

The air around the package is extracted and taken to an analysis chamber containing an IR beam or gas sensor that can detect the presence of target molecules—and therefore micro-holes. This way, it is possible to automatically inspect every single package, avoiding problems of returns and consumer dissatisfaction caused by poor preservation.

IR Spectroscopy and Gas Sensors

The technologies that enable in-line inspection are based on nondispersive infrared technology, which offer rapid response times and reliable measured values. In the case of very small leakages, measurements with very low concentration differences or measurements by means of containers, the technology is based on the principle of laser spectroscopy.

A monochromatic radiation beam emitted by a laser interacts with the gas molecules being measured. The radiation wavelength coincides with one of the absorption lines of the molecule. Measuring the intensity and absorption profile of the radiation with a photodetector makes it possible to detect the presence of a gas, and determine the concentration of the molecule being measured.

For certain gases, the high sensitivity of measurement can be obtained by using a modulation technique of the absorption measurement known as wavelength modulation spectroscopy (WMS). It involves transmitting sinusoidal modulation to the wavelength variation of the laser radiation, then creating a beat between the signal detected from the photodetector and the modulation frequency.

The distinct advantage of WMS is that it eliminates constant contributions to the absorption, such as that of the container, thereby making it possible to significantly increase the sensitivity of the measurement. The realization of gas sensors for application in the pharmaceutical, bottling and food sectors originated at Italy’s University of Padua, where lasers have been employed to create laboratory prototypes for determining the concentration of gas pressure using absorption spectroscopy techniques.

Industrial application of these technologies has brought IR and laser spectroscopy technology to the market and into production lines, improving the way in which quality control is performed on packaged products. The non-destructive measurement techniques, based on absorption spectroscopy, are today finding new areas of use—not only to monitor package leakages, but also to monitor the internal gases and check their evolution during product shelf life.

Case History: An In-line Control of Micro-holes in the Food Industry

Let’s explore an example of micro-hole inspection via IR spectroscopy and gas sensors, and how certain challenges might be overcome.

For one company, micro-hole inspection technology was initially working by detecting molecules leaking from packages being transferred on conveyor belts. However, during the technology transfer stage, it became evident that the pressure difference between inside and outside of the container was not enough to determine the presence of micro-holes at the line’s speed without touching the package.

To combat this, a system of rollers was implemented to apply the correct pressure to force leakage of target molecules, indicating the presence of micro-holes, without damaging the packaging or the product. The rollers are designed to stress the container and the seals to encourage gas to be released in the event of a leak.

The inspection is applicable on trays as well as bags or flowpacks. Packages are inspected at 360°, both on top and at the bottom (including any longitudinal seals) by inserting air extractors also on the sides and under the package, creating a special opening in the conveyor belts.

The target molecules that can be detected with these technologies are numerous, and vary according to the type of preservation mixture. For example, it is possible to detect CO2 as a target molecule for all MAP-preserved products, or alcohol in the case of bakery products, or specific product aromas for products packaged in air or nitrogen.

Practical applications
Examples of practical applications. Figure courtesy of FT System.


The in-line inspection for micro-holes in packaging through the application of IR spectroscopy, or by means of gas sensors, makes it possible to go from spot checks to in-line inspections on 100% of production. The solution can be applied on trays and bags and does not require the internal gas mixture or the line speed to be changed. It can be easily integrated in existing lines and inspection is reliable, precise and repeatable.

This quality control technology has game-changing potential for products preserved in MAP, alcohol or nitrogen, since it makes it possible to check for micro-holes in the packaging and the integrity of the seal on each individual product. From practical experience in the production line, it is evident that all micro-holes are not detected by spot checks.

In addition, a return or recall, for example for the presence of mold in fresh pasta or in cheese due to a micro-hole, causes significant economic and image damage for the company. Implementing this modern application of IR spectroscopy in the line thereby makes it possible to prevent and intervene in real time on the production process to guarantee the integrity of the package and avoid problems related to safety, quality and preservation.

Food Fraud

Food Fraud: How Chemical Fingerprinting Adds Science to the Supply Chain

By Sam Lind, Ph.D.
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Food Fraud

You would be forgiven for thinking that food fraud is a sporadic issue but, with an estimated annual industry cost of $50 billion dollars, it is one currently plaguing the food and drink sector. In the UK alone, the food and drink industry could be losing up to £12 billion annually to fraud.

As the scale of food fraud becomes more and more apparent, a heightened sensitivity and awareness of the problem is leading to an increasing number of cases being uncovered.

Recently: Nine people contracted dangerous Vibrio infections in Maryland due to mislabeled crabmeat from Venezuela; food fraud raids have been conducted in Spain over fears of expired jamon re-entering the market; and authorities seize 1 ton of adulterated tea dust in India.

Spurred by the complexity of today’s global supply chains, food fraud continues to flourish; attractive commercial incentives, ineffective regulation and comparatively small penal repercussions all positively skew the risk-reward ratio in favor of those looking to make an extra dollar or two.

The 2013 horsemeat scandal in Europe was one such example, garnering significant media attention and public scrutiny. And, with consumers growing more astute, there is now more onus on brands to verify the origin of their products and ensure the integrity of their supply chains.

Forensic science is a key tool in this quest for certainty, with tests on the product itself proving the only truly reliable way of confirming its origin and rooting out malpractice.

Current traceability measures—additives, packaging, certification, user input—can fall short of this: Trace elements and isotopes are naturally occurring within the product and offer a reliable alternative.

Chemical Fingerprinting for Food Provenance

Like measuring the attributes of ridgelines on the skin of our fingertips as a unique personal identifier, chemical fingerprinting relies on differences in the geochemistry of the environment to determine the geographic origin of a product—most commonly measured in light-stable isotopes (carbon, nitrogen, sulphur, oxygen, hydrogen) and trace elements.

Which parameters to use (either isotopes, TEs or both) depends very much on the product and the resolution of provenance required (i.e. country, farm, factory): Isotope values vary more so across larger geographies (i.e., between continents), compared to smaller scales with TEs, and are less susceptible to change from processing further down the supply chain (i.e., minced beef).

The degree of uptake of both TEs and light isotopes in a particular produce depends on the environment, but to differing extents:

TEs are related to the underlying geochemistry of the local soil and water sources. The exact biological update of particular elements differs between agricultural commodities; some are present with a lot of elements that are quantifiable (“data rich” products) while others do not. We measure the presence and ratio of these elements with Inductively Coupled Plasma—Mass Spectrometry (ICP-MS) instrumentation.

Light Isotopes are measured as an abundance ratio between two different isotopes of the same element—again, impacted by environmental conditions.

Carbon (C) and nitrogen (N) elements are generally related to the inputs to a given product. For example, grass-fed versus grain-fed beef will have a differing C ratio based on the sugar input from either grass or grain, whereas conventionally farmed horticulture products will have an N ratio related to the synthetic fertilisers used compared to organically grown produce.

Oxygen (O) and hydrogen (H) are strongly tied to climatic conditions and follow patterns relating to prevailing weather systems and latitude. For ocean evaporation to form clouds, the O/H isotopes in water are partitioned so that droplets are “lighter” than the parent water source (the ocean). As this partitioning occurs, some droplets are invariably “lighter” than others. Then, when rainfall occurs, the “heavier” water will condense and fall to the ground first and so, as a weather front moves across a landmass, the rainfall coming from it will be progressively “lighter”. The O/H ratio is then reflected in rainfall-grown horticultural products and tap water, etc. Irrigated crops (particularly those fed from irrigation storage ponds) display different results due to the evaporation, which may occur over a water storage period.

Sulphur (S) has several sources (including anthropogenic) but is often related to distance from the sea (“the sea spray effect”).

Analysis of light isotopes is undertaken with specialist equipment (Isotope Ratio Mass Spectrometry, IRMS), with a variety of methods, depending on product and fraction of complex mixtures.

Regardless of the chemical parameter used, a fingerprinting test-and-audit approach requires a suitable reference database and a set of decision limits in order to determine the provenance of a product. The generation of sample libraries large enough to reference against is generally considered too cost prohibitive and so climatic models have been developed to establish a correlation between observed weather and predicted O/H values. However, this approach has two major limitations:

  1. The chemical parameters related to climate are restricted (to O and H) limiting resolving power
  2. Any model correlation brings error into further testing, as there is almost never 100% correlation between measured and observed values.
    As such, there is often still a heavy reliance on building suitable physical libraries to create a database that is statistically robust and comprehensive in available data.

To be able to read this data and establish decision limits that relate to origin (i.e., is this sample a pass or fail?), the parameters that are most heavily linked to origin need to be interpreted, using the statistics that provide the highest level of certainty.

One set of QC/diagnostic algorithms that use a number of statistical models have been developed to check and evaluate data. A tested sample will have its chemical fingerprint checked against the specific origin it is claimed to be (e.g, a country, region or farm), with a result provided as either “consistent” or “inconsistent” with this claim.

Auditing with Chemical Fingerprints

Chemical fingerprinting methods do not replace traditional traceability systems, which track a product’s journey throughout the supply chain: They are used alongside them to confirm the authenticity of products and ensure the product has not been adulterated, substituted or blended during that journey.

A product can be taken at any point in the supply chain or in-market and compared, using chemical fingerprinting, to the reference database. This enables brands to check the integrity of their supply chain, reducing the risk of counterfeit and fraud, and, in turn, reducing the chance of brand damage and forced product recalls.

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