AOAC 133rd Annual Meeting - Final Program

Poster Abstracts | Wednesday

P-W-029 Landon Wiest , Paul Connolly , Joe Konschnik , Restek Corp., Bellefonte, PA, USA The Analysis of Acrylamide Using an Aqueous Compatible Reversed-Phase Column by LC-MS/MS Detection Acrylamide is a byproduct of the Maillard reaction when alde- hyde sugars and the amino acid asparagine react at elevated temperatures. Acrylamide can be found in foods such as 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 repro- ductive 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 regu- lation, there has been an increase in need for chromatographic determination of acrylamide in foods. Leading LC-based chro- matographic methods that quantify acrylamide often suffer from irreproducibility and poor column lifetimes. This results in longer turnaround times, less instrument uptime, and poor data qual- ity. A new method has been developed that addresses both pain points that utilizes a reproducible, retentive, and robust analyt- ical column. The benefits of the new method will be discussed showing examples of difficult matrices such as coffee and potato products with particular emphasis on the role of the analytical column on the success of the analytical method. Presenter: Landon Wiest, Restek Corp., Bellefonte, PA, USA, Email: landon.wiest@restek.com ANALYSIS OF NON-FOODBORNE CONTAMINANTS AND RESIDUES P-W-030 Fatjon (Anthony) Hanelli , Douglas Stevenson , Chad Nelson , NuSkin Enterprises Inc., Provo, UT, USA Mass Spectrometry Approaches for Identifying Contaminants and Adulterants in Dietary Supplements Fitness nutrition, weight management and herbal dietary supple- ments are a major part of the dietary-supplements industry and they are targets for adulteration and ingredient-labeling inac- curacies. Adulteration with prohibited anabolic steroids and/or stimulants is either intentional, or inadvertent, as a result of poor manufacturing processes. Manufacturers and quality-assurance testing agencies need to develop strategies to comprehensively detect and identify a wide range of possible contaminants and adulterants in order to assure their absence. A strategy to identify anabolic steroid agents and stimulants in various types of supplements is presented, in which analyses with advanced mass spectrometry techniques are key. Mass spectrometry-based strategies initially involve a “non-targeted” approach to accu- rately screen for a broad range of potential contaminants and adulterants. High-resolution and high mass accuracy mass spectrometry (Q-ToF) is essential for screening, and components are identified with a high-degree of confidence based on several

mass spectral criteria, as well as searches against databases and comparison with authentic standards. Subsequently, methods have been developed for routine monitoring and quantitation of these now known “targeted” contaminants and adulterants using either LC-MS/MS (Q-ToF), LC-MS/MS (triple-quad) or SFC/ MS, which can provide greater efficiency and throughput. Presenter: Fatjon (Anthony) Hanelli, NuSkin Enterprises Inc., Provo, UT, USA, Email: ahanelli@nuskin.com P-W-031 Hui Zhou , Ying Qi , Lih-Wen Ding , Chad Nelson , Douglas Stevenson , Nu Skin Enterprises, Provo, UT, USA A Mass Spectrometry Survey of Polycyclic Aromatic Hydrocarbon (PAH) Contamination in Botanical Extracts Polycyclic aromatic hydrocarbons (PAHs) are a class of compounds containing carbon, hydrogen, and multiple aromatic rings. PAHs originate from burning substances and are found throughout the environment. Most are considered carcinogenic. Botanical materials often contain PAHs due to environmen- tal exposure or uptake from contaminated water, air, or soil. PAH contamination can also occur from over-heating or other processing steps during material preparation. The maximum allowable levels for PAHs in foodstuffs in the European Union has been set to 50 ppb (EU No. 2015/1933) for the sum of four PAHs (i.e., benzo[a]pyrene, benz[a]anthracene, benzo[b]fluo- ranthene, and chrysene), with a maximum for benzo[a]pyrene of 10 ppb for dietary supplements containing botanical ingredients. A mass spectrometry-based method (GC/MS/MS) has been developed and validated for analysis of the four regulated PAHs, as well as other PAHs, in botanical extracts. More than 20 differ- ent botanical and fungal species from different suppliers (e.g., black rice, willow bark, and green tea) have been analyzed for PAHs, with a wide range of findings. Multiple extraction methods and solvent systems were compared, and specific methods were found to be critical for efficient recovery of PAHs for different sample types (e.g., botanicals and fungi). PAHs were identified at different stages of processing, from growing and harvesting, to extraction and manufacturing. Presenter: Hui Zhou, Nu Skin Enterprises, Provo, UT, USA, Email: hzhou@nuskin.com P-W-032 Michael Young , Melvin Blaze , Waters Corp., Milford, MA, USA Before the introduction of the highly sensitive and selective LC-MS instrumentation commonly used for today’s multi-resi- due methods, compound or class specific analytical methods were required to meet regulatory requirements. These methods often involved cumbersome and time-consuming multi-step analyte isolation and enrichment followed by cumbersome and time-consuming multi-step cleanup. With modern instru- mentation, sample preparation for residue analysis requires far less time and analytical complexity. A simple extraction procedure followed by a simple cleanup step (dispersive SPE Optimization of a Pass-Through SPE Cleanup Protocol Prior to LC-MS/MS Multi-Residue Veterinary Drug Analysis

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