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AOAC 2019

133rd AOAC Annual Meeting & Exposition

Restek at AOAC 2019
Restek at AOAC 2019

SCIENTIFIC SESSIONS

New Blood 2019: Developing Methods for the Detection of Important Chemical Analytes, Residues, and Contaminants
Optimizing GC-MS and GC-MS/MS Analysis of 3-MCPD and Glycidyl Esters
Jana Rousova
Restek Corporation
For more information, email Jana Rousova.
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3-MCPD and glycidyl esters in edible oils are contaminants that are formed through refining processes, and several of these substances have been classified as possible human carcinogens. Methods, which are similar to one another, have been developed by ISO, AOCS, and DGF for analyzing these contaminants. While the methods cover extraction and derivatization techniques in detail, very little attention is paid to the GC-MS methods. With emerging automated systems, it is important to simplify and speed up the method by optimizing the parameters, including a switch to split injection. The initial optimization of the temperature program led to an 8-minute decrease in the analysis time and additional time can be saved by utilizing free method development software. The employment of split injection resulted in better peak shape and achieved limits of detection that were comparable to splitless injection. Further evaluation of split injection revealed that the same performance is achieved regardless of inlet temperature, resulting in greater flexibility for different inlet configurations.

Certified Reference Materials: Advancements in Manufacturing and Stability
Unlocking the Mystery of Pesticide CRM Stability for Food Analysis
Joe Konschnik
Restek Corporation
For more information, email Joe Konschnik.
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There is a growing global need for pesticide residues testing in a wide variety of food commodities. In response to this need, testing laboratories must develop versatile analytical methods and workflows in order to produce scientifically sound results which ensure the safety of our food. One of the many challenges faced by food chemists is acquiring suitable pesticide certified reference materials (CRMs) to calibrate analytical equipment, monitor method performance, and confirm the identity and concentration of pesticide residues. Questions regarding the stability of pesticide CRMs abound among users and there is a need to educate and inform the community. CRM producers invest considerable resources to ensure the stability of their products. The authors will discuss ISO standard 17034 requirements to properly manufacture, package, and ensure the stability of pesticide CRMs. Proper CRM handling and storage practices in the lab will also be presented as guidance to ensure stability. The results of pesticide stability studies will be presented showing what can be expected after ampuls are opened and mixed together for routine use.

RESTEK TECHNICAL POSTERS

Analysis of Acylglycerols in Edible Oils by Gas Chromatography Using a Unique Stationary Phase
Presenter: Joe Konschnik
Restek Corporation
For more information, email Joe Konschnik.
Download a PDF of the full presentation.
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Characterization of edible oils is essential to the food industry due to the amount of fraudulent activity that surrounds these products. Some edible oils (e.g., extra virgin olive oil) carry high value, making it an attractive target for fraud. By mixing different vegetable oils (e.g., rapeseed, sunflower, etc.) with high quality olive oils, manufactures and suppliers increase their oil yields and make larger profits on counterfeit olive oils. For these reasons, it is important to obtain a triacylglycerol (TAG) fingerprint of edible oils to know that they have not been adulterated. In addition, the freshness of oils can be determined by looking at the ratio of 1,2 to 1,3-diacylglycerols (DAG). By using a unique gas chromatography (GC) stationary phase without bleed interference and retention time shifting due to phase loss, one is able to resolve TAGs and DAGs, and a full analysis of the edible oil can be conducted for oil adulteration and degradation. The analysis and results for these oils will be presented along with an examination of column bleed at high GC operating temperatures.

The Analysis of Mycotoxins in CBD Oils by LC-MS/MS
Presenter: Ashlee Gerardi
Restek Corporation
For more information, email Ashlee Gerardi.
Download a PDF of the full presentation.
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Mycotoxins, secondary metabolites produced by fungi, are among the most toxic contaminants in cannabis and other agricultural products, capable of causing disease and death in humans and other animals. In the analysis of mycotoxins, using immunoaffinity columns (IACs) to reduce matrix effects and eliminate potential sources of interference for LC-MS/MS analysis is common. When not used, significant matrix interferences have been shown to elute near target mycotoxins, resulting in an adverse effect on measured ion ratios. Herein, alternatives to IACs including dilute-and-shoot, dispersive solid phase extraction (dSPE), and pass-through SPE are evaluated and applied to the analysis of aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2, and ochratoxin A in commercially available CBD oils by LC-MS/MS.

Quantitation of Mycotoxins in Four Food Matrices Comparing Stable Isotope Dilution Assay (SIDA) with Matrix-Matched Calibration Methods by LC-MS/MS
Presenter: Joe Konschnik
Restek Corporation
For more information, email Joe Konschnik.
Download a PDF of the full presentation.
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Mycotoxins are secondary fungal metabolites produced by mold that may be found in food or feed. They can cause severe health problems in humans and animals, and can result in significant economic losses. Among the hundreds of toxic mycotoxins, aflatoxins, fumonisins, deoxynivalenol, ochratoxin A, HT-2 toxin, zearalenone, and T-2 toxin are considered as a major concern for corn, wheat, peanuts, and other agricultural products. LC-MS has become the standard approach and is now widely used for routine mycotoxin analysis and identification. One of the challenges faced by LC-MS techniques is the matrix effects caused by the use of electro-spray ionization (ESI). Generally, sample preparation, chromatographic conditions, and calibration techniques are the common strategies for reducing the negative impacts of matrix effects. Standard addition, matrix matching, and stable isotope dilution assay (SIDA) are all possible calibration solutions. In this work, a quick “dilute-filter-shoot” method was used for sample preparation. A seven-minute LC-MS/MS method using a biphenyl phase column was developed and verified for quantifying 12 mycotoxins in four commodities: corn, peanut butter, brown rice, and mixed corn and wheat. Both SIDA and matrix-matched calibration methods were applied, compared, and evaluated in terms of recovery, efficiency, advantages, and limitations.

The Analysis of Acrylamide Using an Aqueous Compatible Reversed-Phase Column by LC-MS/MS Detection
Presenter: Landon Wiest
Restek Corporation
For more information, email Landon Wiest.
Download a PDF of the full presentation.
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Acrylamide is a byproduct of the Maillard reaction, which occurs when aldehyde sugars and the amino acid asparagine react at elevated temperatures. Acrylamide can be found in roasted coffee and starchy foods, such as potato chips, toasted bread, and cereal. Studies on lab mice have shown that excessive ingestion of acrylamide can result in neurological and reproductive side effects. Acrylamide has also been classified as a category 1B carcinogen, having caused cancer in animal testing. With these risks, regulations have been put in place in the European Union and a Prop 65 warning was issued in California regarding acrylamide. With health concerns and added regulation, there has been an increase in need for chromatographic determination of acrylamide in foods. Leading LC-based chromatographic methods that quantify acrylamide often suffer from irreproducibility and poor column lifetimes. This results in longer turnaround times, less instrument uptime, and poor data quality. A new method has been developed that addresses both pain points by utilizing a reproducible, retentive, and robust analytical column. The benefits of the new method will be discussed showing examples of difficult matrices (coffee and potato products) with particular emphasis on the role of the analytical column on the success of the analytical method.

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