Automated determination of EU Water Framework Directive priority contaminants in surface water at pg/L detection limits using Stir Bar Sorptive Extraction (SBSE) GC/MS/MS

Highly sensitive determination of around 100 contaminants at trace concentrations
from low double-digit to low triple-digit pg/L was performed in surface water. Priority
compounds from the EU water framework directive (EU-WFD) as well as substances
from other legislations were included. A sequential stir bar sorptive extraction (SBSE)
approach employing the GERSTEL Twister was used for analyte enrichment from 100
mL water samples. The Twister was thermally desorbed, compounds were separated
via GC and detected by tandem mass spectrometry (MS/MS) utilizing the highly
sensitive Agilent 7010 Mass Spectrometer with High Efficiency Source (HES).
The analysis method was comprehensively validated to meet the requirements of
the EU-WFD for inland surface water. Repeat analysis of water samples spiked at
concentrations close to the LOQs of the respective analytes demonstrated relative
standard deviations between 1 and 15 % with an average of 6.9 %. (n=6) Trueness
was mainly between 90 and 110 % with an average of X. The correct quantitation of
particle-adsorbed compounds like PAHs was examined and confirmed using certified
reference sediment.
Cypermethrin, heptachlor, heptachlorepoxide and also dicofol in other surface waters
were the only compounds for which the required LOQs could not be reached. To date
there is no technique known to the authors that reaches the required LOQs of 0.06
pg/L for heptachlor and heptachlorepoxide. The developed analysis method was
successfully applied to real world water samples.
Surface water analysis is a critical part of quality control, with the EU leading the world in setting limits for a wide range of contaminants. Those countries outside of the EU could also benefit from being able to offer a high quality, Agilent and GERSTEL supported solution for water analysis.
– Background on Legislation for EU Water Framework Directive
– Basics on Twister and Thermal Desorption Unit (TDU)
– Application Description on Agilent/GERSTEL VAR-Solution
– Product Placement and Positioning
– Competition Analysis

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