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Automated method to determine pharmaceutical compounds in wastewater using on-line solid-phase extraction coupled to
César Augusto Marasco Júnior1, Bianca Ferreira da Silva1,2, Rafaela Silva Lamarca1
1National Institute for Alternative Technologies of Detection, Toxicological Evaluation and Removal of Micropollutants and Radioactives (INCT-DATREM), Institute of Chemistry, São Paulo State University, P.O. Box 355, Araraquara, SP, 14800-060, Brazil.
An automated method using on-line solid-phase extraction (SPE) and LC-MS/MS efficiently detects pharmaceutical compounds in wastewater. This rapid, reliable technique is ideal for environmental monitoring and routine analysis.
Area of Science:
- Environmental Chemistry
- Analytical Chemistry
Background:
- Pharmaceutical compounds are emerging contaminants in wastewater.
- Accurate quantification of these compounds is crucial for environmental risk assessment.
Purpose of the Study:
- To develop and validate an automated method for determining pharmaceutical compounds in wastewater.
- To enable routine environmental monitoring with high sensitivity and efficiency.
Main Methods:
- On-line solid-phase extraction (SPE) coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS).
- Method validation according to international guidelines, including MDL, MQL, linearity, precision, and matrix effects.
- Isotope dilution calibration to minimize matrix effects.
Main Results:
- The automated method achieved rapid analysis (24 min run time) with high precision (intra-day <10%, inter-day <17%).
- Method detection limits (MDL) ranged from 1x10^-6 to 1 μg/L, and quantification limits (MQL) from 0.001 to 3 μg/L.
- Caffeine was the most frequently detected compound in wastewater samples (up to 715 μg/L).
Conclusions:
- The developed automated on-line SPE-LC-MS/MS method is suitable for routine analysis of pharmaceutical compounds in wastewater.
- The method offers high efficiency, minimal sample handling, and reliable results for environmental applications.
- It provides a robust tool for monitoring pharmaceutical pollution in aquatic environments.
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