# Dual Ionization Ion-Mobility Mass Spectrometry Hyphenated with Catalytic Oxygenation-Mediated Extraction

## TL;DR

This paper introduces a new method combining two ionization techniques with a low-cost ion-mobility mass spectrometer to analyze volatile compounds in complex liquids.

## Contribution

The novel integration of APCI and SESI with COME IM-MS enables analysis of diverse VOCs in liquid matrices.

## Key findings

- The system provides 2D separation at low cost using a custom-built ion-mobility spectrometer and commercial triple quadrupole MS.
- Ethyl acetate was successfully extracted and analyzed from complex matrices like Taiwanese millet wine and whiskey.
- An isotopically labeled internal standard improved consistency across multiple analyses.

## Abstract

Catalytic oxygenation-mediated extraction (COME) is an
environmentally
friendly liquid–gas extraction technique that generates oxygen
microbubbles via the catalytic decomposition of hydrogen peroxide.
While corona discharge atmospheric pressure chemical ionization (APCI)
is widely used for analyzing moderately polar and lower-polarity analytes
with low molecular weights, secondary electrospray ionization (SESI)
is a soft ionization technique that effectively ionizes polar volatile
analytes. This study aims to integrate APCI and SESI with COME drift-tube
ion-mobility (IM) triple quadrupole mass spectrometry (MS) to analyze
volatile organic compounds (VOCs) with different physicochemical properties
present in liquid matrices. The coupling of a house-built ion-mobility
spectrometer with a commercial triple quadrupole mass spectrometer
provides 2D separation at low cost. The user can choose one of the
two ionization modes to achieve high signals with VOCs of different
polarity. COME was applied to extract ethyl acetate from complex matrices
(Taiwanese millet wine and whiskey) for immediate IM-MS analysis.
An isotopically labeled internal standard was used to compensate for
drift time and intensity shifts across multiple analyses. The system
operates automatically with a graphical user interface enabling immediate
ion-mobility spectrum visualization for targeted m/z.