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Chromatography Theory and Applications: A Virtual Symposium - Day 1 - Gas Chromatography
ZÁZNAM | Proběhlo Čt, 22.10.2020
V této dvoudenní online akci budou řečníci diskutovat o teorii a aplikacích plynové chromatografie (GC) a vysoce účinné kapalinové chromatografie (HPLC).

In this two-day online event, speakers will discuss theory and applications of gas chromatography (GC) and high performance liquid chromatography (HPLC). We have a morning and afternoon session each day, plus a lunchtime tutorial session on 2D-GC on Day 1. There will be live Q&A for the morning sessions and the tutorial. Attendance is free.

Morning session: 10am EDT – 11:30am EDT: Gas Chromatography Theory and Applications, I

Session chair: Emanuela Gionfriddo (Assistant Professor, Department of Chemistry, Biochemistry, University of Toledo)

10:00 am Welcome and Introductions
10:05 am Natural or Synthetic? Determining the Integrity of Flavors and Fragrances for Consumer Products with GC–MS—An Example from the Analysis of Lavender Essential Oil

Lavender essential oil contains linalool and linalyl acetate as major components. Our studies showed that some commercial lavender samples contain unidentified trace molecules (linalool oxide acetate cis trans furanoids), which we later confirmed as markers of synthetic linalyl acetate. Before confirming that the markers indicated the presence of the synthetic linalyl acetate, three possible scenarios were considered for the marker molecules: 1, that they were process-derived or auto-oxidized artifact molecules; 2, that they were natural compounds; and 3, that synthetic linalyl acetate had been added. In this talk, I explain the analytical process we followed, using gas chromatography–mass spectrometry (GC–MS) methods, to explore these hypotheses.

Presenter: Prabodh Satyal, PhD (Chief Scientific Officer, Aromatic Plant Research Center (APRC))

10:25 am FAME Analysis:Solvent-Mediated (SM) Covalent Adduct Chemical Ionization (CACI-)MS/MS for Complete Assignment of Double Bond Position Using Triple-Quadrupole Mass Spectrometry

Double bond location, along with geometry and chain branching, are the key structural elements determining fatty acid function, but are not available from conventional electrospray tandem mass spectrometry (MS/MS) or by any widely available MS technique applied to fatty acid methyl esters (FAME). Nearly 20 years ago we introduced chemical Ionization (CACI-)MS/MSbased on an ion-molecule reaction between CH2=C=N+=CH2 derived from an CH3CN self-reaction and neutral FAME and developed it for location of double bonds in most unsaturated FAME at GC rates. We report modification of a commercial triple-quadrupole MS instrument that enables high sensitivity CACI-MS/MS enabled by solvent-mediated chemical ionization (SM-CI). We used a prototype SM-CI gas inlet system consisting of a pressurized flow inlet for low volatility solvents. Using the CACI-MS/MS approach, M+54 ions were tested for a wide range of homoallylic FAME with 1-6 double bonds, with monoenes of unknown double bond position derived from cell culture experiments with genetically modified human cells, and with conjugated polyenes derived from seed oil extracts. We also looked at signal response consistency for quantitative analysis. We discuss the results of this study, which demonstrate that the novel source enables structural assignments without standards for nearly all unsaturated fatty acids, offering the sensitivity advantages of a triple-quadrupole MS instrument for high sensitivity applications, including true selected ion monitoring.

Presenter: J. Thomas Brenna, Professor (Depts. of Pediatrics, of Chemistry, and of Nutrition, The University of Texas at Austin, and Cornell University, Ithaca, New York, USA)

10:45 am Identifying Key Drivers of Toxicity in Drinking Water: Sensitive GC–MS Methods Push the Envelope

This study identifies important drivers of toxicity for disinfection by-products (DBPs) in drinking water. DBPs are by far the dominant organic contaminants found in drinking water, are formed by the reaction of disinfectants with natural organic matter (NOM) and are an untended consequence of trying to make water microbially safe to drink. However, DBPs are linked to several adverse effects, including bladder cancer, miscarriage, and birth defects. Our goal is to understand which DBPs are the drivers of toxicity so that they can ultimately be minimized in drinking water. For this research, improved analytical methods using gas chromatography–mass spectrometry (GC–MS) were developed, allowing ng/L quantification limits for nearly 60 priority, unregulated DBPs with different chemical properties. Many of these compounds are more toxic than the DBPs currently regulated. Drinking water samples from across the United States were studied, including those with saltwater intrusion and wastewater impacts. Results revealed that regulated DBPs were not the big drivers of toxicity, but that several priority, unregulated DBPs are. Our study highlights the power of highly sensitive GC–MS methods and how they can be used to improve the safety of drinking water.

Presenter: Susan Richardson, Arthur Sease Williams Professor of Chemistry, University of South Carolina

11:05 am Question-and-answer (Q&A) period with all speakers in the session

Lunchtime tutorial session: 12:30–1:30 pm EDT

12:30 - 1:30 pm EDT TUTORIAL: From Petroleum to Cannabis—Comprehensive Two-Dimensional Gas Chromatography (GC×GC) Solutions for Complex Sample Analysis

One-dimensional gas chromatography (GC) analysis is challenging for many petroleum, cannabis, food, environmental, and biological samples. The massive amounts of components with a wide range of concentrations results in numerous overlapping peaks. It is often difficult to achieve fundamental knowledge about the sample, discover impurities, or identify indicative biomarkers without further separation. While emphasis has been placed on mass spectrometry (MS) to achieve another dimension of separation, comprehensive two-dimensional gas chromatography (GC×GC) has proven successful when 1D GC-MS is insufficient. There is an outstanding need to educate and inform the broad analytical community about the established technique of GC×GC. This tutorial session will provide examples of the successful implementation of GC×GC to overcome obstacles in complex sample analysis. Specifically, the talk will explain:

  • the benefits of GC×GC for challenging sample analysis
  • fundamental operation and considerations of GC×GC systems
  • resources for method development and data processing with GC×GC

Presenter: Michelle Misselwitz, Chemist Consultant, Chemistry Matters Inc.

Michelle Misselwitz is an environmental chemist consultant with Chemistry Matters. Chemistry Matters, a niche consulting company, specializes in using GC×GC for industrial clients and forensic investigations. Previously, Michelle developed GC×GC solutions to support the environmental, food safety, petroleum, and botanical analysis markets. Michelle has taught over 15 professional seminars and hands-on courses on the subjects of gas chromatography (GC), mass spectrometry (MS) and sample preparation. She has 10 years of experience with GC×GC, including 5 years of daily operation. Through education efforts and promoting tangible benefits, Michelle is passionate about increasing widespread adoption of GC×GC.

Afternoon session: 2pm EDT – 4pm EDT: Gas Chromatography Theory and Applications, II

2:00 pm Welcome and Introductions
2:05 pm Comprehensive Analysis of Cannabis Using Two-Dimensional Gas Chromatography with High Performance Time-of-Flight Mass Spectrometry (GCxGC–TOF-MS)

Hemp characterization is not only important for determining its legality in the United States, but also critical for determining the effectiveness and safety of its many products. Regrettably, reported test results are often incomplete or inaccurate. In this study, gas chromatography–mass spectrometry (GC–MS) and comprehensive GCxGC–MS technology were used for untargeted analysis of cannabis botanicals. The methodology included pesticide analysis, potency determination, and terpene profiling. Data collection was comprehensive; however, both targeted and untargeted data processing methods were utilized for the quantitative and qualitative analysis of samples. The analytical methodology provided data with superior chromatographic resolution and increased peak signal to noise values, which dramatically improved compound detection and identification. Enhanced chromatographic plots and high-performance TOF-MS facilitated chemical classification and differentiation of cannabis samples.

Presenter: David E. Alonso, PhD, Applications Chemist, LECO Corporation, St. Joseph, Michigan

David E. Alonso was born in Fort Riley, Kansas, and then moved to the Chicago area where he spent most of his youth. He obtained his BS in chemistry from Andrews University and his PhD in organic chemistry from the University of Notre Dame. He has taught chemistry at Andrews University, and is currently an applications chemist at LECO Corporation in St. Joseph, Michigan. His work currently focuses on metabolomics, forensics, and environmental analysis.

2:25 pm Rapid Rinse and Shoot: A Screening Method for Pesticides in Fruit by GC–MS in Under Six Minutes

A gas chromatography-mass spectrometry (GC–MS) system has been configured for fast screening of residual pesticides present on the surface of fruits. The method uses a GC oven with direct heating technology and mass spectrometry (MS) spectral deconvolution. Residual pesticides are rinsed from the tested commodity surface with acetone. The rinsate is collected and injected into the GC–MS system. The direct heating oven allows a very high temperature program rate (250 °C/min) to complete the GC–MS analysis in 3.4 minutes. Deconvoluted spectra are searched against a user created library and NIST 17 using retention indices for time filtering, resulting in rapid and confident identification of pesticides present on the fruit. The entire analysis from sample rinsing to reporting takes under 6 minutes. This talk will describe application of the method to fresh fruits. The approach is particularly useful for prioritizing samples (triage) for more in-depth analysis.

Presenter: Bruce D. Quimby, PhD (presenter), Senior GC/MS Applications Scientist, and Anastasia A. Andrianova, PhD, GC/MS Applications Scientist, both at Agilent Technologies, Inc., Wilmington, Delaware

Bruce Quimby is a Senior Applications Scientist in the Mass Spectrometry Division of Agilent Technologies, located in Wilmington, Delaware. He received a Ph.D. in analytical chemistry from the University of Massachusetts (Amherst) in 1980 and a bachelor’s degree in chemistry from Mansfield State College (PA) in 1974. He has been at Agilent Technologies (formerly Hewlett-Packard) since 1979, working the first 10 years in research and development. He has authored or co-authored 18 journal articles and 16 patents in the field of gas chromatography and mass spectrometry. He is currently working in GC/MS applications in multiple areas.

2:45 pm Use of Barrier Discharge Ionization Detection for the Analysis of Water in Liquefied and Gaseous Petroleum Samples

Barrier discharge ionization detection for gas chromatography (GC-BID) is a novel universal detector capable of detection of nearly any volatile analyte with the exception of helium and neon. Traditional analyses of moisture in hydrocarbon samples are labor intensive and error prone. Here we will explore the use of GC-BID for detection of moisture (water) in liquified petroleum gas and gaseous hydrocarbon samples. It is critical to understand the moisture content of hydrocarbon mixtures as it will affect their processing characteristics and utility as fuels. GC-BID coupled with an ionic liquids column has proven to be an easy and reliable method of separating and quantifying trace (ppm) levels of water in those samples.

Presenter: Allison Mason (presenter), Product Manager, System Gas Chromatography, Ian Shaffer, Product Specialist, Gas Chromatography, Andrew Fornadel, Marketing Manager, Energy and Petrochemicals, all at Shimadzu Scientific Instruments

Allison Mason earned her BS in chemistry from the University of Maryland, Baltimore County. She went on to earn her MS in Physical Chemistry from the University of California, Irvine. Allison started her career in chromatography as a service engineer working with custom valve gas chromatography in 2012. She joined Shimadzu in 2016 and was promoted to System GC Product Manager in 2018.

3:05 pm Qualitative Analysis of Meat Aroma with SPME-GC­–MS

Solid-phase microextraction (SPME) is a solvent-less extraction technique which makes use of a sorbent fiber to ad/absorb compounds from a headspace or liquid sample. Headspace SPME improves selectivity and sensitivity for volatile compounds and reduces matrix effects. Because aroma is responsible for most of what we know as flavor, looking at volatile odorants is critical for any food product. This work describes the development of a SPME-GCMS method suitable for qualitative analysis of cooked-meat aroma, and an optimization of several different fiber coatings to assess the wide range of odorants present in cooked-meat.

Presenter: Madeleine DiGregorio, GCMS Product Specialist at Shimadzu Scientific Instruments

Madeleine Y. DiGregorio, PhD (née Bee), is currently a GCMS Product Specialist at Shimadzu Scientific Instruments. She received her BS in Chemistry from American University and her PhD in Food Science from Cornell University with Dr. Gavin Sacks. Her doctoral research focused on the developed of a high-throughput, trace-level approach for quantitative aroma analysis in wine grapes using direct analysis in real time (DART)-MS in collaboration with E&J Gallo Winery.

3:25 pm Low-Pressure Gas Chromatography (LPGC)–The Fast Way to Your Pesticide Analysis

Saving time while ensuring the same level of performance is a goal of every analytical chemist. The technique of gas chromatography under low pressure (LPGC), or near vacuum GC, can provide that for your analysis. In this webinar, we will explain how this technique works and what the advantages and drawbacks are. We will then discuss its application to the analysis of pesticides in food commodities.

Presenter: Jana Rousova, Applications Scientist, Restek

Jana Rousova, PhD, is an application scientist in Restek’s innovations laboratory. Her primary research focus is the development of solutions in food analysis for GC–MS and GC–MS/MS. Jana has over 10 years of experience with method development both gas and liquid chromatography. Prior to joining Restek, she received her PhD in analytical chemistry from the University of North Dakota and MS degree at the University of Chemical Technology in Prague.

3:45 pm How to Determine if a Gas Generator is Right for Your Laboratory

As laboratories continue to seek new ways to streamline sampling, decrease costs and improve efficiencies, the thought of incorporating a gas generator to support key instruments is often visited. Without first identifying a few key drivers including gas costs, personnel, lab expansion plans and so forth, it is difficult to accurately determine if the decision is best for your plans. The following step by step guide as proven helpful for many existing users that followed prior to their decision.

  • Determine the Instruments You Want to Support
  • Identify the Associated Costs of Gases and Transportation
  • Get the Endorsement of the Instrument Company
  • Chose a Known Manufacturer
  • Chose a Partner for the Life of the Gas Generator
  • Compare the Dollars & Sense

Presenter: Jack Mahan (Sales Manager, North America, Parker Analytical Gas Systems)

Jack Mahan is the Global Sales Manager, Analytical Gas Systems for the Industrial Gas Filtration and Generation Division of Parker Hannifin. He received a B.S. in Business Administration and Marketing from Fitchburg State University, Fitchburg, MA and an MBA from Nichols College, Dudley, MA. Jack has over 31 years of experience in the life science market, focusing on laboratory instrumentation including Liquid Chromatography/Mass Spectrometry, Gas Chromatography, Nuclear Magnetic Resonance, Fourier Transform Infrared Spectroscopy and Total Organic Carbon Analyzers.

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