Vortex-assisted surfactant-enhanced emulsification liquid–liquid microextraction for the determination of carbamates in juices by micellar electrokinetic chromatography tandem mass spectrometry

• A MEKC–MS/MS method is proposed for determination of 25 carbamates in juice samples.
• A sample treatment based on VSLLME has been optimized.
• A (semi)volatile surfactant (APFO) is used in the extraction and as BGE.
• LOQs are below maximum residue levels allowed by EU in processed food.
• The proposed method is a good alternative for carbamate determination in juices.

A new method based on vortex-assisted surfactant-enhanced-emulsification liquid–liquid microextraction has been developed for the extraction of carbamate pesticides in juice samples prior to their determination by micellar electrokinetic chromatography coupled to tandem mass spectrometry. This sample treatment allowed the satisfactory extraction and the extract clean-up of 25 carbamates from different fruit and vegetal juices (banana, tomato, and peach). In this study, the addition of ammonium perfluorooctanoate in the aqueous sample in combination with vortex agitation, provided very clean extracts with short extraction times. Under optimized conditions, recoveries of the proposed method for these pesticides from fortified juice samples ranged from 81% to 104%, with relative standard deviations lower than 15%. Limits of quantification were between 2.3 µg kg−1 and 4.7 µg kg−1, showing the high sensitivity of this fast and simple method.

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