Tag Archives: gas chromatography

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Natural Goes Methodical

By Susanne Kuehne
No Comments
Susanne Kuehne, Decernis
Food fraud
Find records of fraud such as those discussed in this column and more in the Food Fraud Database, owned and operated by Decernis, a Food Safety Tech advertiser. Image credit: Susanne Kuehne

The popularity of “natural” foods with consumers has increased exponentially over the past decade or two. While the term “natural” on a food label is not formally regulated by the FDA, “natural flavors” have been defined in the Code of Federal Regulations Title 21 as flavoring constituents derived from a naturally occurring source, such as spice, fruit, vegetable, herb, leaf and more. “Natural” flavors/aromas have specific spectroscopic fingerprints versus synthetically produced volatile organic compounds. This method combines gas chromatography and isotope ratio mass spectroscopy (GC-C-IRMS) to determine whether a fruit aroma is naturally or synthetically-derived, and can be used to build a database of natural flavors.

Resource

  1. Strojnik, L., et al. (July 5, 2021). “Construction of IsoVoc Database for the Authentication of Natural Flavours”. MDPI Open Access Journals.
Katie Banaszewski, NOW Foods
In the Food Lab

Making Supplements Safer: Tackling the Pesticide Problem

By Katie Banaszewski
No Comments
Katie Banaszewski, NOW Foods

Precise, accurate contaminant analysis is crucial to ensure that dietary supplements are of high quality and free from potentially harmful chemicals, such as heavy metals or pesticide residues. As supplements become an increasingly prevalent part of global health culture, with their global market forecast to reach a value of more than $230 billion by 2027, there is an urgent need to ensure their safety for consumers—but manufacturers face many challenges in this area.

Assuring that dietary supplements are free of pesticide contamination is especially difficult given their botanical ingredients, which can be more complex than other analytes. A prominent obstacle is matrix interference. As most botanical ingredients exist in the form of concentrated extracts, smaller sample sizes are needed to overcome heavy matrix interference, in turn requiring highly sensitive instrumentation to detect minute amounts of pesticide residues.

With this in mind, we adopted an analytical workflow comprising both gas and liquid chromatography (GC and LC) systems for orthogonal residue analysis. GC-MS/MS can achieve fast, robust separation of ~300 pesticide residues, while LC-MS/MS enables analysis of ~280 residues. The GC and LC instruments are sufficiently sensitive to allow dilution of samples to mitigate matrix interference— essential to determine potentially low residue levels in complex matrices, and ensure dietary supplements can confidently be certified safe.

Clearing Analytical Hurdles

Matrix complexity is only increased by the fact that botanical ingredients are sourced from across the world and, therefore, exposed to many different agricultural practices. As a wide range and great many of these botanical ingredients are used to produce supplements, it is challenging to develop sample preparation procedures that are suitable for all products.

To prevent frequent iterations of analytical procedures, we developed one sample preparation workflow for GC-MS/MS and another for LC-MS/MS. In both, samples are hydrated and extracted (using acetonitrile:water and the salts anhydrous magnesium sulfate and sodium chloride) before cleanup by solid-phase extraction (SPE). For LC, various defined combinations of dispersive SPE analysis are used to accommodate different matrices (pigmented, high-fat or high-protein, for example) before samples are diluted prior to analysis. Doing so allows us to optimize sample preparation for particular groups of botanical matrices and target specific matrix mitigation without needing to change the entire workflow.

In addition to the aforementioned analytical hurdles, some lesser-defined commodities lack maximum residue limits, complicating the interpretation of results and specification of acceptable criteria. To mitigate these difficulties, we opted to streamline our data processing and reporting by implementing integrated chromatography data system software for both LC-MS/MS and GC-MS/MS. This enables on-the-spot evaluation of QC criteria and rapid assessment of component presence (or absence) in data review and facilitates swifter and easier cGMP compliance.

Keeping Supplements Safe

Our chosen analytical approach has created robust, sensitive processes for optimized multi-residue analysis of dietary supplement samples in a regulated QC environment.

With uptake of supplements fast increasing, guaranteeing product safety is more important than ever. Improved pesticide screening, and quality control of food ingredients, holds great value for both individual organizations and the industry as a whole, while—crucially—enabling consumers to rest assured about the safety of the products available to them.

Susanne Kuehne, Decernis
Food Fraud Quick Bites

Criminals in the Lab

By Susanne Kuehne
No Comments
Susanne Kuehne, Decernis
Testing methods, analysis
Find records of fraud such as those discussed in this column and more in the Food Fraud Database. Image credit: Susanne Kuehne

Herbs and botanical ingredients are a common target for fraud, especially during times of increased demand, for example caused by COVID-19. The Botanical Adulterants Prevention Program (BAPP) published an article describing some of the fraudulent methods that are used to intentionally create false results. The paper explains how deliberately manipulated plant extracts can fool lab methods like gas chromatography or high-performance liquid chromatography to produce results which make the analyzed product look legitimate.

Resource

  1. Nutraceuticals World. (October 30, 2020). “BAPP Publishes Article Detailing Adulteration Schemes Used to Fool Laboratory Analytical Methods”.
Schimadzu, GCMS-QP2020

Shimadzu Releases High-Sensitivity GCMS Instrument for Labs

By Food Safety Tech Staff
No Comments
Schimadzu, GCMS-QP2020

Shimadzu Scientific Instruments has announced the availability of a GCMS-QP2020 high-sensitivity gas chromatograph mass spectrometer. With custom configurations to meet the demands of food labs, the instrument features a multi-function ion source, high-speed scan control and a large-capacity turbomolecular pump with heightened exhaust efficiency, which improves instrument performance when operated using helium, hydrogen and nitrogen. The mass spectrometer’s ion source technology creates a stable space for ion creation, prevents contamination due to source interactions, and offers the ability to switch ionization modes without venting the system. Users can employ a Quick-CI option that enables the introduction of reagent gas while using the EI source to look for the molecular ion. A smart selected ion monitoring (SIM) functionality enables higher SIM sensitivity. Additional features included upgraded GCMSsolution software for intuitive control of the mass spectrometer. Optional databases have additional retention indices for common columns and support accurate qualitative analysis, quantitative method development and screening studies.