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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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In inductively coupled plasma–mass spectrometry (ICP–MS), an inductively coupled plasma (ICP) torch is used as an atomizer and ionizer. Solid samples are dissolved and volatilized before being introduced into the high-temperature argon plasma, while solution samples are nebulized and passed through the high-temperature argon plasma. Plasma dissociates the analytes and ionizes their component atoms to form a mixture of positive ions and molecular species. The positive ions are then...
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The mass analyzer is a crucial component of the mass spectrometer. In the ionization chamber, the vaporized sample is bombarded with a high-energy electron beam to generate a radical cation and further fragment into neutral molecules, radicals, and cations. A series of negatively charged accelerator plates accelerate the cations into the mass analyzer. The mass analyzer separates ions according to their mass-to-charge (m/z) ratios and then directs them to the detector. The common types of mass...
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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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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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Sample Preparation for Probe Electrospray Ionization Mass Spectrometry
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A Small Footprint and Robust Interface for Solid Phase Microextraction and Mass Spectrometry Based on Vibrating

Jing Wang1, Chong Li1, Peng Li1

  • 1C. Eugene Bennett Department of Chemistry, West Virginia University, Morgantown, West Virginia 26506, United States.

Journal of the American Society for Mass Spectrometry
|January 18, 2022
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Summary

A novel interface integrates solid phase microextraction (SPME) with capillary vibrating sharp-edge spray ionization (cVSSI) for mass spectrometry (MS). This portable system enables rapid, sensitive drug analysis from serum with minimal solvent and time.

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Area of Science:

  • Analytical Chemistry
  • Separation Science
  • Mass Spectrometry

Background:

  • Solid phase microextraction (SPME) coupled with mass spectrometry (MS) is vital for bioanalytical, environmental, and forensic applications.
  • Existing SPME-MS methods require efficient interfaces for sample handling and analyte ionization.
  • Expanding SPME-MS scope necessitates convenient and integrated coupling solutions.

Purpose of the Study:

  • To develop and demonstrate a novel integrated interface for SPME-MS analysis.
  • To combine desorption and ionization steps into a single device using capillary vibrating sharp-edge spray ionization (cVSSI).
  • To showcase the system's capability for rapid and sensitive quantification of drug compounds.

Main Methods:

  • A capillary vibrating sharp-edge spray ionization (cVSSI) device was designed for in-situ nebulization.
  • SPME probes were inserted into the cVSSI capillary for direct desorption and ionization.
  • The integrated interface was tested for drug compound analysis in serum samples.

Main Results:

  • The cVSSI interface successfully coupled SPME desorption with MS ionization.
  • Rapid MS analysis of drug compounds (metoprolol, capecitabine, etc.) from serum was achieved.
  • Excellent linearity (R² = 0.97-0.99) and low limits of detection (0.25-0.59 ng/mL) were obtained using minimal solvent (3.5 μL) and time (3 min).

Conclusions:

  • A portable, cost-effective SPME-MS interface was demonstrated.
  • The integrated cVSSI system offers high sensitivity, short analysis times, and a small footprint.
  • This technology is suitable for various sample cleanup applications, including drug monitoring, environmental, and forensic analysis.