Reliability of Multi-residue Identification

It is of utmost importance to ensure that the analytical results from residue testing for food products are reliable. “False positive” findings of hazardous residues in food result in safe product being rejected and leading to potential huge financial and juristic implications. “False negative” findings result in contaminated product being on the shelf and increase the risk of a foodborne disease. The reliability of testing results depends on the type of methodology and the performance criteria. Identification is the important step before a residue is reported. Procedures for identification should be rigorous and depend on sensitivity and selectivity of the MS techniques. The causes of “false positive” and “false negative” derived from both QqQ-MS and HR-MS detection will be discussed. The approaches of establishing a “fit-for-purpose” methodology and identification criteria for both QqQ-MS and HR-MS will be introduced. This will help the testing labs build the protocols/procedures to follow to reduce the incidence of “false detections”; help set up the criteria for identification; and help deliver the highly accurate results.

 

Hui Zhao
Pre-Sales Application Engineer
Agilent Technologies, Inc.

 

Hui has 13 years of industry experience developing and validating analytical methods for food/feed nutrition, food safety, dietary supplements and botanicals testing, using a variety of analytical techniques including LC-TQ, LC-QTOF, LC-DAD and GC-MS and a breadth of sample preparation methodologies. She has worked as a Research Scientist at Monsanto, EPL-Bioanalytical Services, Tate & Lyle, Inc. and Lead Staff Scientist at Covance Food Solutions. She holds a Master of Science degree in Analytical Chemistry from Lanzhou University in China and a Ph.D. in Analytical Chemistry from the University of Missouri.

Prior to becoming a Pre-Sales AE, Hui worked as an LCMS application scientist in Agilent’s global market development group where her primary focus was food and environmental market development.

 

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Aqueous Film Forming Foam Formulations

Aqueous film forming foam (AFFF) is an effective fire suppressant for petroleum-based fires.  Foams are primarily composed of complex mixtures of per- and polyfluorinated substances (PFAS), but the exact composition is protected business information.  Identification of PFAS using High–resolution mass spectrometry (HR-MS) only utilizes the accurate mass and isotope pattern of the molecular ion and is not robust as formulas do not provide structural information.  Fragment ions from MSMS spectra can greatly improve identification confidence with software tools such as Fluoromatch. Data-dependent acquisition (DDA) is a common tool used to acquire MSMS spectra when the composition is unknown.  In this study, three approaches based on DDA acquisition for the MSMS fragmentation of fluorinated compounds were optimized and compared.

 

Emily Parry, PhD
LC/MS Applications Scientist
Agilent Technologies, Inc.

 

Emily Parry received her PhD degree in Environmental Chemistry from the University of California, Davis. She joined Agilent after completing her postdoctoral work at the Environmental Protection Agency (EPA). Her specialty is method development and measurement of emerging contaminants.

 

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Dioxins Analysis in the Environment

U.S. EPA Method 1613B has been one of the primary methods used in the analysis of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) in wastewater, soils, sludges, and other matrices. These compounds have more than 200 congeners, and seventeen of them are highly toxic and of interest in trace analysis. Historically, these analyses have been performed using magnetic sector high-resolution GC/MS. In 2021, the U.S. EPA approved an alternate testing protocol (ATP) that accepts GC/TQ as an equivalent technology for the analysis of dioxins in environmental samples.  This work shows the Agilent triple quadrupole GC/MS system can achieve the sensitivity required to meet and exceed guidance for the analysis of PCDD/PCDFs at all concentration levels.

 

Joel Ferrer
Product Manager – Agilent QQQ GC/MS
Agilent Technologies, Inc.

 

Joel Ferrer is the Product Manager for the Agilent Triple Quadrupole GC/MS portfolio. He obtained his B.S. in Biomedical Sciences at Texas A&M University where he gained experience on Agilent LC/MS and GC/MS instrumentation performing metabolomics research in the Department of Chemistry. Joel later earned his MBA from the University of Houston with a focus in Product Management and Marketing Analytics. He’s been with Agilent for over 5 years and in his current product management role since June 2020.

 

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High-Throughput Intact Native Protein Analysis

Ion mobility-mass spectrometry has become a valuable analytical tool in native protein analysis. In protein structure studies, ion mobility spectrometry provides rotationally averaged collision cross-section values that correlate to size and shape of the biomolecule. For proteins, ground state CCS and accurate mass are not adequate to identify different proteins. Therefore, the introduction of gas phase unfolding followed by ion mobility measurements provide unique fingerprints for native protein analysis. This collision-induced unfolding (CIU) technique can be utilized to identify proteins and protein complexes. Typical CIU experiments utilize static nano-ESI or standard ESI using a syringe pump for sample introduction which is difficult to automate. In this study, we have developed a new automated sample introduction method for high-throughput CIU experiments which can be adapted for IgG and other proteins.

 

Sheher Banu Mohsin, Ph.D.
Senior Applications Scientist
Agilent Technologies, Inc.

 

Sheher Mohsin is a senior applications scientist at Agilent Technologies. She received her Ph. D in physical chemistry from the University of Illinois and an MBA from Rockhurst University. She started her career at the US Environmental Protection Agency working on dioxin analysis with high-resolution mass spectrometers. She later joined Bayer and worked in the special analysis lab using mass spectrometry to solve problems in synthesis, impurity determination and submission of final product impurity profile to regulatory agencies. Sheher’s current focus is on lipidomics using GC, LC and SFC separations and mass spectrometry. Sheher collaborates with academic and government researchers working on complex problems to come up with innovative, simplified workflows using the latest tools in separation and mass spectrometry.

 

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HydroInert for Use with Hydrogen Carrier Gas

Recent concerns with the price and availability of helium have led laboratories to look for alternative carrier gases for their GC/MS and GC/MS/MS systems. For GC/MS, hydrogen is the best alternative to helium. Among the problems encountered when converting to hydrogen carrier gas in GC/MS is that hydrogen is not an inert gas and may cause chemical reactions in the mass spectrometer electron ionization (EI) source. This can lead to disturbed ion ratios in the mass spectrum, spectral infidelity, and peak tailing. Therefore, a novel EI source for GC/MS and GC/MS/MS was developed and optimized for use with hydrogen carrier gas.

To evaluate the novel EI source performance, several classes of compounds including SVOCs, VOCs, PAHs, PCBs, phthalates, and pesticides were analyzed with GC/MS and GC/MS/MS using hydrogen as the carrier gas. The results demonstrated:

  • Good spectral fidelity for compounds susceptible to hydrogenation in the source resulting in higher library match scores observed against the NIST spectral library when compared to the conventional EI source. This effect was especially pronounced for nitrobenzene and other nitro-compounds
  • Excellent chromatographic peak shape, especially for late-eluting PAHs with a fast analysis method that is known to amplify any chromatographic peak tailing
  • Good performance for the analysis of over 200 pesticides with both GC/MS and GC/MS/MS
  • Dramatically improved calibration performance for SVOCs
  • Excellent spectral matching and calibration performance for VOCs analyzed with headspace in drinking water
  • Demonstrated excellent sensitivity at the sub-ppb level for many analytes including PAHs and PCBs, exceeding that typically seen with hydrogen carrier gas with both GC/MS and GC/MS/MS
  • Stable system performance for over 5,000 injections of a heavy soil extract.

The novel EI source addresses one of the operational issues impacting the environmental laboratory industry with using hydrogen as the carrier gas.

 

Anastasia A. Andrianova
GC/MS Application Scientist
Agilent Technologies, Inc.

 

Anastasia Andrianova is a GC/MS Applications Scientist in the Mass Spectrometry Division of Agilent Technologies, located in Wilmington, Delaware. She received a Ph.D. in analytical chemistry from the University of North Dakota (Grand Forks) in 2017 and a combined masters’ and bachelor’s degree in analytical chemistry from the Moscow State University (Moscow, Russia) in 2014. Anastasia has been at Agilent Technologies since 2018. She has authored or co-authored over 30 journal articles and application notes, as well as 1 patent in the field of analytical chemistry, focusing on chromatography and mass spectrometry. Anastasia is currently working in GC/MS applications in multiple areas with a focus on food and environmental analysis.

 

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Optimised Analysis of SVOCs with EPA 8270E

This webinar will overview a sensitive method used to analyse semivolatile organic compounds (SVOCs) on an Agilent 7000E Gas Chromatograph/Triple Quadrupole (GC/TQ) Mass Spectrometer. The utilization of GC/TQ instrumentation for analysis of SVOCs offers significant advantages:

  • Excellent selectivity afforded by Multiple Reaction Monitoring (MRM) mode results in faster batch review and increased confidence due to the elimination of matrix interferences often present when using GC/MS acquisition modes; and
  • Better sensitivity enables smaller extraction volumes which improves sustainability, reduces waste, and decreases costs associated with sample preparation, solvent usage, and waste disposal.
  • Key analytical techniques which facilitated this work will be discussed.
  • Manufacturer’s recommended tune protocol for mass accuracy and resolution checks in accordance with US EPA Method 8270E will also be discussed.

 

Rachael Ciotti
GC/MS Application Specialist
Agilent Technologies, Inc.

 

Rachael Ciotti is a GCMS Application Specialist at Agilent Technologies in Wilmington, DE. Previously, she was a Field Service Engineer specializing in installing, maintaining, and repairing Agilent GC and GC/MS systems. Prior to joining Agilent, Rachael worked at DuPont as an analytical chemist responsible for GC and GC/MS method development and transfer to manufacturing labs. She holds a Bachelor of Arts in Mathematics from Rutgers University.

 

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Knowing How to Make ICP-MS Easier

Knowing the right information at the right time can help you cut through the everyday complexities of your ICP-MS analysis.

Driven by insights from customers from around the world, Agilent has developed a range of Easy-fit supplies, intuitive yet powerful software and complete workflows to bring the confidence of knowing you will get the answers you need to efficiently run your lab.

Watch the presentation and learn how to make your ICP-MS applications easier to run, maintain and control.

 

What you will learn

  • Learn how our range of Easy-fit supplies can simplify your workflow
  • Discover our selection tools that can help you get your ICP-MS configured right for your analysis
  • Take a look at ICP-MS MassHunter software
  • Learn about some of the simple software tools and time-saving tips that can help you get the very best out of your ICP-MS.

 

Gareth Pearson
ICP-MS Supplies Product Manager (Agilent, Spectroscopy Technology Innovation Centre, Melbourne, Australia)

Angie is a proteomics scientist on the application team at Evosep BioSciences. Her work focuses on bringing standardization, throughput, and depth into translation proteomic research studies. During her PhD at University College Dublin studying proteomics in inflammatory arthritis and postdoc at Cedars Sinai, Los Angeles, Angie conducted large scale biomarker studies, where she gained considerable experience with the Evosep One and the Agilent triple quadrupole mass spectrometers.

 

Gareth Pearson
ICP-MS Supplies Product Manager (Agilent, Spectroscopy Technology Innovation Centre, Melbourne, Australia)

Angie is a proteomics scientist on the application team at Evosep BioSciences. Her work focuses on bringing standardization, throughput, and depth into translation proteomic research studies. During her PhD at University College Dublin studying proteomics in inflammatory arthritis and postdoc at Cedars Sinai, Los Angeles, Angie conducted large scale biomarker studies, where she gained considerable experience with the Evosep One and the Agilent triple quadrupole mass spectrometers.

 

Gareth Pearson
ICP-MS Supplies Product Manager (Agilent, Spectroscopy Technology Innovation Centre, Melbourne, Australia)

Angie is a proteomics scientist on the application team at Evosep BioSciences. Her work focuses on bringing standardization, throughput, and depth into translation proteomic research studies. During her PhD at University College Dublin studying proteomics in inflammatory arthritis and postdoc at Cedars Sinai, Los Angeles, Angie conducted large scale biomarker studies, where she gained considerable experience with the Evosep One and the Agilent triple quadrupole mass spectrometers.

 

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Novel Front-end Strategies to Increase Sample Throughput in LC/MS

Imagine if you could perform ‘LC/MS’ analysis in a comparable time to Usain Bolt’s 100-metre world record!  Over the last 15 years through iterative technological product enhancements and by the replacement of a traditional UHPLC with a simple sample cleanup step, the RapidFire system has accelerated MS analyses in many fields ranging from HTS, ADME, biopharma, synthetic biology, food, and the life sciences.

However, sometimes when there is an unavoidable requirement for good chromatographic separation, then an alternative, low-cost strategy exploiting Ultra-Fast LC can be adopted to reduce analysis times from minutes to seconds. This webinar presents the new RapidFire400 system for HTS and will contrast its analytical merits to the complimentary Ultra-Fast LC approach.

 

What you will learn

•    How the RapidFire400 meets the needs of  today’s high throughput requirements
•    Learn how a standard Agilent LC can be configured to the Ultra-Fast LC mode
•    Understand the advantages and limitations of both high sample throughput strategies

 

Andreas Mielcarek
Pre-Sales Applications Scientist
Agilent

 

Andreas Mielcarek is a pre-sales Applications Scientist with Agilent Technologies. He has been with Agilent for 5 years developing LC, RapidFire, and mass spec methods on a wide range of molecules. Prior to joining Agilent, he worked as a LC-MS Core-facility scientist at the University Marburg, were he obtained his PhD in bioanalytical chemistry.

 

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Ultra-High Sensitivity for Targeted Mass Spectrometry Applications

The Evosep One is a powerful and standardized platform for LCMS workflows that require a sensitivity boost achieved at low flow rates between 100nl/min to 4ul/min. The robustness and throughput of the standardized methods on the Evosep One combined with the sensitivity of the Agilent 6495C triple quadrupole support targeted analysis of proteomes with ultra-high sensitivity down to the single cell level.

We demonstrated this by targeting selected peptides in a complex background of sub-nanogram material and generated dilution curves spanning several orders of magnitude. To ensure seamless integration of the Evosep One with the Agilent 6495C triple quadrupole, we have developed a native driver for MassHunter and a robust solution for the Agilent nanoflow ion source.

 

 What you will learn

•    The application of the Evosep One chromatography system to high-throughput analysis of large cohorts.
•    How there is a growing demand for high throughput and standardized workflows to allow  the  analysis of increasingly large cohorts of samples for proteomic research
•    How high sensitivity is achieved for the accurate measurement of low abundant biomarkers
•    How the Evotip was designed to improve efficiency and recovery associated with sample purification and loading ahead of MS analysis.

 

Angela McArdle
Evosep Senior Scientist
Evosep Biosystems

 

Angie is a proteomics scientist on the application team at Evosep BioSciences. Her work focuses on bringing standardization, throughput, and depth into translation proteomic research studies. During her PhD at University College Dublin studying proteomics in inflammatory arthritis and postdoc at Cedars Sinai, Los Angeles, Angie conducted large scale biomarker studies, where she gained considerable experience with the Evosep One and the Agilent triple quadrupole mass spectrometers.

 

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Adding an Extra Dimension of Separation

With the increasing demand for high throughput LC/MS analyses, there is a temptation to reduce chromatographic run times, but in some instances, this can give rise to significant interferences, thus compromising the result. Or perhaps, despite improvements in column resolution you still observe a reduction in sensitivity and selectivity due to ion suppression or elevated background noise caused by matrix effects? Could it be that you need to carry out discovery work and need to confidently identify ‘unknown’ compounds using a high-resolution MS strategy?

Maybe all your analyses could benefit from further separation of sample components?

We will discuss the 6560C Ion Mobility LC/Q-TOF system and explain how it exploits ion mobility as an extra dimension of separation to increase feature coverage whilst reducing background noise to avoid losses in sensitivity. An exemplary workflow detailing a bona fide 4-dimensional LC/MS method to characterize compounds including proteins without increasing analytical run times will be described.

 

 What you will learn

•    The principles and benefits of ion mobility (IM) and how it can help multiple applications
•    How adding an orthogonal gas phase separation (IM) allows faster chromatography to be used to separate isobars and matrix components
•    How accurate Collisional Cross Sections (CCS) values from drift time measurements delivers higher confidence for untargeted workflows
•    How to separate and characterize different protein conformers present in a single solution

 

Hannah Florance
Application Scientist
Agilent

 

In 2006, Hannah gained her PhD at the University of Edinburgh in non-covalent protein interactions in solution and the gas phase under the tutelage of Prof. Perdita Barran.

Hannah is currently an LC/MS applications specialist for Agilent, based in Cheadle, UK and has had multiple roles in the life sciences research, starting as a protein chemist, before moving into the proteomics and metabolomics fields.

 

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