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Updated: Jun 27, 2026

High-throughput and Comprehensive Drug Surveillance Using Multisegment Injection-Capillary Electrophoresis-Mass Spectrometry
Published on: April 23, 2019
Multisyringe flow injection system for solid-phase extraction coupled to liquid chromatography using monolithic
Hugo M Oliveira1, Marcela A Segundo, José L F C Lima
1Faculdade de Farmácia, REQUIMTE, Serviço de Química-Física, Universidade do Porto, Porto, Portugal.
This study introduces a rapid, automated solid-phase extraction method coupled with HPLC-UV for detecting priority phenolic pollutants in water at ng/mL levels, offering a reliable tool for environmental monitoring.
Area of Science:
- Environmental Chemistry
- Analytical Chemistry
Background:
- Phenolic compounds are priority pollutants in water, necessitating sensitive detection methods.
- Existing methods for phenolic pollutant analysis can be time-consuming and complex.
Purpose of the Study:
- To develop a fast, automated solid-phase extraction (SPE) procedure for screening priority phenolic pollutants in water.
- To achieve low limit of detection (LOD) and high enrichment factors for phenolic compounds.
Main Methods:
- A flow-through column SPE system utilizing a polystyrene-divinylbenzene sorbent was integrated with a multisyringe flow injection system (MSFIA).
- The MSFIA system was computer-controlled for automated sample loading and analyte elution, directly coupling sample preparation to HPLC-UV determination.
- Enrichment factors, LODs, and recovery rates were evaluated for phenol and ten derivatives in various water matrices.
Main Results:
- High enrichment factors (mean value 176 for 50 mL sample) were achieved for phenolic pollutants.
- Limit of detection (LOD) values below 1 ng mL(-1) were obtained for the maximum sample volume (100 mL).
- Mean recoveries ranged from 89% to 103% across different water matrices, with successful validation using certified reference material.
Conclusions:
- The developed automated SPE-HPLC-UV method is a fast, reliable, and sensitive tool for water quality and environmental monitoring of phenolic pollutants.
- The system demonstrates high efficiency in sample preparation and analyte determination, suitable for routine analysis.
- The method's applicability was confirmed through successful testing with certified reference materials and contaminated soil samples.
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