Development of an environment-friendly microextraction method for the determination of aliphatic and aromatic aldehydes in water

• A sensitive and robust alternative for analysis of aldehydes as DBPs by GC–MS.
• A fast and simple microextraction method for simultaneous extraction/derivatisation of up to 13 aldehydes.
• LVI coupled to PTV for improving the sensitivity and selectivity of the method.
• An environment-friendly methodology to monitor aldehydes as DBPs in water.

Aldehydes are produced in water disinfected primarily by ozone treatment, and are generally present in treated water below the limit of detection (<5 μg L−1) of commonly proposed methods. Formaldehyde is the most studied along with acetaldehyde due to their mutagenic character, and because it causes chromosomal aberrations. This paper reports the first miniaturised system for the simultaneous determination of thirteen aldehydes (aliphatic and aromatic) which are selected based on their frequent or suspected presence in water, mainly as disinfection by-products (DBPs). The micro liquid–liquid extraction (MLLE) method is a miniaturisation of EPA Method 556.1 for carbonyl compounds that includes some innovations, such as performing the derivatising reaction in a strong acidic medium (pH 1.1), and the addition of magnesium sulphate to the aqueous layer as the heating agent, which allows to carry out the whole simultaneous derivatisation/microextraction process in only 1 min. Large-volume sample injection (50 μL) coupled to programmed temperature vaporiser–gas chromatography–mass spectrometry is also used to improve both sensitivity and selectivity. The MLLE method demonstrated high extraction efficiency (96%) with low limits of detection, between 0.7 and 80 ng L−1, and good precision (RSD below 10%, n = 11). The proposed method was evaluated by determining aldehydes in water. Our study demonstrated that the selection of the target aldehydes was appropriate since all were found (at average concentrations from 8.0 to 1.4 μg L−1 for aliphatic and aromatic aldehydes, respectively) in swimming pool waters as DBPs.

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