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For the first time, we coupled a microextraction technique using a magnetic ionic liquid with voltammetric determination. A hydrophobic magnetic ionic liquid that contains the tetrachloromanganate(II) anion, namely, aliquat tetrachloromanganate(II), was synthesized and used for the extraction of ascorbic acid from aqueous solutions followed by voltammetric determination. The extraction procedure was carried out using a single drop microextraction technique in which the ascorbic acid containing magnetic ionic liquid was separated with a magnet and then cast onto the surface of a carbon paste electrode modified with TiO2 nanoparticles for the voltammetric quantification of the extracted ascorbic acid. Electrochemical quantification was carried out in a blank phosphate buffer solution. After optimizing different experimental conditions, a linear concentration range of 1.50-40.0 nM with a detection limit of 0.43 nM was obtained for the determination of ascorbic acid. The presented approach was successfully applied to the determination of ascorbic acid in samples of vitamin C effervescent tablets and orange juice. [ABSTRACT FROM AUTHOR]