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8th International Symposium on Recent Advances in Food Analysis

RAFA
RAFA

RESTEK PRESENTATIONS


VENDOR SEMINAR

Soft Solutions to Hard Problems: Saving Time and Money in the Laboratory with the EZGC Web Tools
Dr. Hansjoerg Majer (presenter), Jonathan Keim, Chris Rattray, Chris English
Restek Corporation
For more information, e-mail Hansjoerg Majer.
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Analytical laboratories face continual pressure to increase productivity while decreasing costs. With recent advances in available technology, we can find valuable opportunities to save time and money by using GC simulation software to quickly optimize methods from our desks instead of in the lab. In this talk, we will share work showing how the EZGC suite of online tools can be used to improve gas chromatographic analyses. We will show several examples of how the free software can be used for method development. Additionally, these tools can be used to improve existing methods in various ways, such as maintaining high-quality separations with much shorter columns, optimizing the splitless valve time, and switching carrier gases.

TECHNICAL POSTERS

Analysis of 648 Pesticides in Foods by LC-MS/MS Utilizing the Raptor Biphenyl Column
Dr. Hansjoerg Majer1 (presenter), David R. Baker2, Neil Loftus2, Laetitia Fages3,
1Restek Corporation, 2Shimadzu Corporation, 3Phytocontrol
For more information, e-mail Hansjoerg Majer.
Download a PDF of the full presentation.
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There are more than 1,000 pesticides used globally on soil and crops. With the ever-increasing international trade within the food industry, regulatory bodies around the world have increased the number of regulated pesticides and the maximum residue levels (MRLs) allowed in food commodities. National pesticide monitoring programs create new challenges for food safety laboratories as the number of pesticides required for analysis is increasing together with an expanded range of food products. In this poster, we present the development of an LC-MS/MS method using a Raptor Biphenyl LC column for screening and quantifying over 646 pesticides in a single analysis. To evaluate the method, QuEChERS extracts of mint, tomato, and apple were provided by a commercial laboratory as raw acetonitrile extracts and spiked with 646 pesticides prior to analysis. The method was evaluated in matrix to ensure that the reporting limits were in agreement with recognized MRLs.

Applying High-Speed Gas Chromatography for the Speciation of Fats in Foods and Edible Oils
Dr. Hansjoerg Majer (presenter), Rebecca Stevens, Jaap de Zeeuw, Jason Herrington
Restek Corporation
For more information, e-mail Hansjoerg Majer.
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Determination of total fat content and its speciation as saturated, unsaturated, polyunsaturated, and trans fat for nutritional labeling is primarily accomplished by derivatization of the hydrolyzed free fatty acids as methyl esters (FAMEs) followed by high-resolution GC-FID analysis. In particular, AOAC method 996.06 describes sample preparation procedures and a GC-FID method for speciation of fats in a variety of food products. Due to the high complexity and very small structural difference between analytes in a typical FAMEs sample, the preferred GC columns are 100 m or longer and use a highly polar cyanopropyl stationary phase. As a result, the associated GC methods are quite slow; AOAC 996.06 requires over an hour of GC analysis time per sample, not including oven cooldown.

The analysis of FAMEs has become increasingly important to food science in recent years. Unsaturated and polyunsaturated fat content is perceived favorably by consumers who, as a whole, are rapidly becoming more conscious of nutritional value. At the same time, the US FDA has issued a final determination that partially hydrogenated oils (those that commonly contain trans fats) are not GRAS and thus cannot be used in food products without specific approval. Fatty acid profiles are also useful in determining origin, authenticity, and sensory attributes of edible oils by chemical fingerprinting.

This work explores using shortened narrow bore columns, high carrier gas flows, and fast oven temperature programming as routes to reduce GC run times for FAMEs analysis. The tradeoff between separation performance and analysis time is explored with the conclusion that relatively complex mixtures of FAMEs can be separated with greatly reduced analysis time.

Achieving Fast and Efficient Separations Using Superficially Porous Particle Column Technology
Joe Konschnik (presenter), Frances Carroll, Sharon Lupo, Shun-Hsin Liang, Ty Kahler, Paul Connolly, Rick Lake, Rob Freeman, Carrie Sprout
Restek Corporation
For more information, e-mail Joe Konschnik.
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Superficially porous particles (SPP) have been proven to provide fast and efficient separations. These particles feature a solid, impermeable core enveloped by a thin, porous layer of silica that decreases the diffusion path and reduces peak dispersion. When combined with highly selective stationary phases, the result is a significant improvement in efficiency and sensitivity compared to fully porous particles (FPP) of similar dimension.

Through various experiments, we hope to demonstrate the advantages of SPP columns over columns packed with traditional 5 µm and 3 µm FPP particles. When used in the development of new assays, SPP particles allow fast run times and excellent method performance without changes in instrumentation. The performance of SPP particle columns will be demonstrated on a variety of applications, including aflatoxins, pesticides, and veterinary drugs. Analysis time, signal-to-noise ratio, and resolution will be evaluated in these experiments.

The versatility of these columns makes them ideal for separations in animal health, food safety, and other testing areas. For example, when analyzing toxic substances in agricultural matrices, such as aflatoxins in wheat, speed is of paramount importance. Four aflatoxins can be eluted in less than 1.5 minutes using ammonium formate and formic acid modified mobile phases and mass spectrometry detection.

Restek LC columns offer the speed of superficially porous particles with the resolution of the highly selective stationary phases, allowing peak separation and faster analysis times to be achieved without expensive UHPLC instrumentation.

Pesticide Residue Analysis in Cannabis Using Modified QuEChERS and LC-MS/MS
Joe Konschnik1 (presenter), Justin Steimling1, Julie Kowalski2, Jeffrey Dahl3, Derek Laine2
1Restek Corporation, 2Trace Analytics, 3Shimadzu Scientific Instruments
For more information, e-mail Joe Konschnik.
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The legal cannabis industry is exploding in the United States as more states adopt medical and recreational use laws. Cannabis is still federally illegal, so the legal cannabis market is managed by local state governments. While systems for growing, production, and sale of cannabis and cannabis-related products are somewhat established, regulation and enforcement of quality and safety testing have lagged behind. Now state governments and private labs are focusing on product safety testing with special emphasis on pesticide analysis. This is the result of various product recalls, media attention, and concern from patient advocacy groups.

Herein, a modified QuEChERS LC-MS/MS method for the analysis of multiresidue pesticides was developed. The AOAC QuEChERS method was used for a reduced 1.5 g amount of plant material and processed with universal dSPE. LC-MS/MS analysis used constant polarity switching ESI and monitored at least two transitions per analyte. Matrix-matched calibration was used for quantitation and both method and instrument internal standards were used. Analyte recovery validation was performed according to FDA guidelines by testing three matrices at three fortification levels in triplicate for over 200 pesticides. For the large majority of pesticides, in all three matrices and at all three fortification levels, recovery was between 70–120%.


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