In-syringe magnetic stirring-assisted dispersive liquid–liquid microextraction for automation and downscaling of methylene blue active substances assay

• Determination of anionic surfactants is automated by in syringe MSA-DLLME.
• The optimal conditions have been determined using a multivariate optimization.
• The method is rapid, sensitive and environmental friendly.
• Water samples of different origin have been successfully analyzed.

A simple and rapid method for the determination of the methylene blue active substances assay based on in-syringe automation of magnetic stirring-assisted dispersive liquid–liquid microextraction was developed. The proposed method proved to be valid for the determination of anionic surfactant in waste, pond, well, tap, and drinking water samples.Sample mixing with reagents, extraction and phase separation were performed within the syringe of an automated syringe pump containing a magnetic stirring bar for homogenization and solvent dispersion. The syringe module was used upside-down to enable the use of chloroform as an extraction solvent of higher density than water.The calibration was found to be linear up to 0.3 mg/L using only 200 µL of solvent and 4 mL of sample. The limits of detection (3σ) and quantification (10σ) were 7.0 µg/L and 22 µg/L, respectively. The relative standard deviation for 10 replicate determinations of 0.1 mg/L SBDS was below 3%. Concentrations of anionic surfactants in natural water samples were in the range of 0.032–0.213 mg/L and no significant differences towards the standard method were found. Standard additions gave analyte recoveries between 95% and 106% proving the general applicability and adequateness of the system to MBSA index determination. Compared to the tedious standard method requiring up to 50 mL of chloroform, the entire procedure took only 345 s using 250-times less solvent.

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