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Mass Spectrometry: Complex Analysis01:21

Mass Spectrometry: Complex Analysis

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Mass spectrometry is an important technique for the identification of pure compounds. However, it has some limitations for the analysis of complex mixtures, often due to excessive fragmentation making the spectrum too complicated to decipher. Mass spectrometry can be combined with suitable separation methods in sequence, forming hyphenated methods, which are useful in the analysis of complex mixtures.
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Mass spectrometry is a powerful characterization technique that can identify and separate a wide variety of compounds ranging from chemical to biological entities, based on their mass-to-charge ratio (m/z). The instruments that allow this detection, known as mass spectrometers, have three components: an ion source, a mass analyzer, and a detector. These spectrometers differ based on the nature of their ion source and analyzers.
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The resolution of a mass spectrometer depends on the efficiency of separating ions with different ion masses. The mass of an atom is approximated to the sum of the masses of protons and neutrons inside, considering the masses of protons and neutrons as equal. However, the masses of the proton (1.6726 × 10−24 g) and neutron (1.6749 × 10−24 g) are not truly equal. There is a minor error in the expression of atomic masses relative to the simplest atom of hydrogen. For...
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Mass Analyzers: Common Types01:19

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The quadrupole mass analyzer consists of four cylindrical metal rods arranged in a diamond carrying a DC voltage and a radio-frequency AC voltage. The motion of ions through the quadrupole depends on the field strength, causing only ions of a certain m/z to resonate successfully and strike the detector at a given field strength. Though the transmission rate for these analyzers is high, the exact elemental composition of the sample is not determined because of low resolution; however, they are...
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Electrospray Ionization (ESI) Mass Spectrometry01:12

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Higher molecular weight biomolecules are nonvolatile compounds that may decompose before ionizing or vaporizing during mass analysis with conventional electron impact ionization methods. Accordingly, electrospray ionization (ESI) is the favored method for vaporizing and ionizing biomolecules as it circumvents rapid fragmentation and enables the recording of mass signals for the entire biomolecule.
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Identifying Per- and Polyfluorinated Chemical Species with a Combined Targeted and Non-Targeted-Screening High-Resolution Mass Spectrometry Workflow
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Multidimensional Separations for Characterization of Isomeric PFAS Using SLIM High-Resolution Ion Mobility and Tandem

Heidi M Sabatini1, Terra Pettit-Bacovin1, Ralph Aderorho1

  • 1Department of Chemistry, Clemson University, Clemson, South Carolina 29634, United States.

Analytical Chemistry
|March 17, 2025
PubMed
Summary
This summary is machine-generated.

Structures for Lossless Ion Manipulations (SLIM)-based high-resolution ion mobility (HRIM) advanced separation of complex per- and polyfluoroalkyl substances (PFAS) isomers. This method enhances identification of emerging PFAS compounds in environmental samples.

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Area of Science:

  • Environmental Chemistry
  • Analytical Chemistry
  • Toxicology

Background:

  • Per- and polyfluoroalkyl substances (PFAS) are persistent synthetic contaminants of global environmental and health concern.
  • Their structural complexity, including isomers and varied functional groups, challenges current analytical methods like high-resolution mass spectrometry (HRMS).
  • Accurate identification and quantification of diverse PFAS in complex matrices require advanced separation techniques.

Purpose of the Study:

  • To demonstrate the efficacy of Structures for Lossless Ion Manipulations (SLIM)-based high-resolution ion mobility (HRIM) for separating complex PFAS isomers.
  • To develop and apply a multidimensional LC-SLIM IM-MS/MS workflow for comprehensive PFAS characterization.
  • To establish methods for identifying emerging PFAS species based on their unique analytical signatures.

Main Methods:

  • Integration of SLIM into a liquid chromatography-ion mobility-mass spectrometry/mass spectrometry (LC-SLIM IM-MS/MS) workflow.
  • Utilizing high-resolution ion mobility (HRIM) for separating branched PFAS isomers.
  • Employing complementary tandem mass spectrometry (MS/MS) techniques, including all ion fragmentation (AIF) and energy-resolved MS/MS.

Main Results:

  • Demonstrated successful separation of complex PFAS branched isomers using SLIM-HRIM.
  • Observed unique arrival time vs. m/z trend lines for sulfonate and carboxylic acid PFAS classes, aiding in emerging species identification.
  • Identified unique fragment ions and fragmentation mechanisms through MS/MS, complementing ion mobility separation.

Conclusions:

  • The combined workflow of chromatography, high-resolution SLIM, and MS/MS offers a powerful approach for identifying unknown PFAS compounds.
  • This advanced analytical strategy is capable of characterizing complex PFAS mixtures in environmental samples.
  • The method provides crucial insights into PFAS structures, aiding in environmental monitoring and risk assessment.