News from LabRulezLCMS Library - Week 34, 2024

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 19th August 2024? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!

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This week we bring to you posters from ASMS 2024 by Agilent Technologies, Shimadzu, Thermo Fisher Scientific, and Waters Corporation!

1. Agilent Technologies: Quantitative Analysis of Legacy & Emerging PFAS in Semiconductor Lubricant using Triple Quadrupole LC/MS

• poster / ASMS 2024

Introduction: Per- and polyfluoroalkyl substances (PFAS) are known to play an important role in the semiconductor industry. For example, PFAS-containing lubricants used in manufacturing processes mainly include perfluoropolyether (PFPE), polytetrafluoroethylene (PTFE) and others that are believed to be of very low toxicity.¹ With environmental regulations & manufacturing restrictions continuing to expand in their scope, the semiconductor industry is facing the challenge of sustainability.² Reliable workflows are needed to ensure effective monitoring and control of PFAS in upstream processes. This study established a workflow based on solid phase extraction (SPE) and LC/MS/MS for analyzing over 100 PFAS from semiconductor lubricant matrix.

Conclusions:

• A reliable workflow for quantitation of trace levels of PFAS in semiconductor lubricant, based on SPE cleanup and LC/MS/MS was developed.
• The Agilent Bond Elut PFAS WAX cartridge offered selective and effective extraction for matrix cleanup and preconcentration of PFAS analytes in lubricant.
• The workflow performance confirmed the applicability of the Agilent PFAS MRM Database and eMethod, for quantitation of PFAS using the Agilent 6475 LC/TQ system.
• This workflow enables a ready-to-use protocol for lubricant suppliers and semiconductor manufactures to monitor trace levels of critical PFAS in lubricants.

2. Shimadzu: Identification of Double Bond Position in Cyclic Ester using OAD TOF system

• poster / ASMS 2024

Overview

Oxygen Attachment Dissociation (OAD) (x1 000 000) is a novel method for fragmentation providing additional fragmentation to CID on the LCMS 9050 To enhance identification of cyclic ester(lactone) which is one of the aromatic ingredients OAD-MS/MS has been applied to provide double bond specific dissociation enabling C=C position assignments.

Introduction: Lactones Lactones, which are aromatic aromatic ingredients find wide applications in perfumes detergents, and foods The aroma is derived from a combination of various compounds rather than single compound The presence of different types and amounts of impurities in these compounds whether synthesized or purified from natural products can result in distinct aromas To accurately evaluate the aroma it is crucial to identify the precise structural information of the compound including impurities However when the compound has a stable cyclic structure such as lactone direct access to the double bond position within the ring by the neutral radical generated through OAD becomes challenging. In this study, various lactones were hydrolyzed to convert the cyclic ester into a hydroxycarboxylic acid, enabling the identification of the double bond position.

Conclusions:

• Hydrolyzation combined with OAD MS/MS was worked to identify C=C bond positions of cyclic ester.
• It was suggested that there are several isomers of Lactone B other than the position of the C=C bond.
• OAD-MS/MS can distinguish isomers that cannot be identified by CID.

3. Waters Corporation: ANALYSIS OF HIGH MASS POLYCYCLIC AROMATIC HYDROCARBONS (PAHS) EXTRACTED FROM MICROPLASTICS SPILLED IN THE MARINE ENVIRONMENT

• poster / ASMS 2024

INTRODUCTION

In 2021 the container ship M/V X-Press Pearl caught fire and later sank off the coast of Sri Lanka. Over 1600 tons of polyethylene pellets, aka nurdles, were aboard the ship along with 25 tons of nitric acid which began to leak and is suspected to be the cause of the fire that lead to the sinking. To add to the witches brew of ingredients in this fire were fertilizers and explosives being transported and flame retardants deployed to douse the fire. When combined with abundant, naturally-occurring compounds found in the marine environment, the need arises to characterize the composition of intact, burned, and broken pieces of the spilled plastic later collected from kilometers of Sri Lankan beaches¹.

Determining the distribution and abundance of PAHs in the samples is important for characterizing the source of the microplastics (MPs) and in selecting appropriate handling, disposal and/or recycling methods. Both traditional and advanced GC/MS methods such as 2D GC are suitable for the determination of PAHs up to 302 Da which is useful for such purposes as the differentiation of pyrogenic versus petrogenic inputs2. However, the toxicity characteristics of samples has demonstrated poor correlation with low mass (<302 Da) PAHs in past studies3. For that reason this work was aimed at investigating the routine analysis of higher mass PAHs in the range of 314 to 424 Da to provide access to additional analytes that may better correlate with toxicity as well as to provide the possibility of additional source markers.

CONCLUSIONS

• Analysis of an expanded range of high molecular weight PAHs in unfractionated extracts of MPs was achieved using a standard GC-APCI QqQ configuration combined with asimple, generic METHODS microextraction
• Charge transfer, atmospheric pressure chemical ionization facilitated the implementation of a class-specific MRM acquisition scheme
• Only minor modification to the GC method used for lower mass PAHs is required
• Nitrogen carrier gas achieved elution of HWM PAHs with symmetric, narrow peaks through the use of flow programming
• Further investigation of HMW PAHs for potential source markers and toxic compounds is enabled with this approach

4. Thermo Fisher Scientific: Carbon and Nitrogen Positional Isotopomer Determination in Metabolites using Orbitrap IQ-X and Stellar MS - a novel hybrid nominal mass instrument

• poster / ASMS 2024

Abstract

Purpose: Development of a targeted MS²/MS³ approach for the determination of positional isotopomers.

Methods: Initial data acquired on Thermo Scientific Orbitrap IQ-X Tribrid Mass Spectrometer was used for the structural annotation. A targeted MSn based assay utilizing the above data to get the structural information of the metabolites was developed on a novel hybrid nominal mass instrument.

Results: A targeted MS²/MS³ method was established for the determination of positional isotopomers in Adenosine Monophosphate (AMP). The method was used for evaluation of the effect of hypoxia on cellular metabolism in an in-vitro model.

Conclusions

• A workflow for targeted stable isotope analysis of isotopomer is described.
• The use of product scans with MSn and alternate fragmentation can give positional information of label using nominal mass resolution instrument.