Large-volume electric field-assisted multiphase extraction of malachite green from water samples: A multisample device and method validation.

In this work, a new large-volume multiphase, multi-sample electroextraction device was developed and applied to selectively extract malachite green (MG) from water samples. This device was easily constructed with ordinary materials and capable of extracting ten samples simultaneously, obtaining MG preconcentrated on a solid support, to fit into a pipette tip. A multi-well plate was applied to extract MG from aquaculture water samples, and the extracts containing the desorbed MG were analysed by LC-DAD and LC-MS/MS. The signals from both detectors were used in two independent validation procedures. Linearity, matrix effect, selectivity, precision, trueness, and limits of detection and quantification were all evaluated. For both detectors, linearity was demonstrated in the range of 0.5-5 µg L-1 (R2 > 0.98). Matrix effect was insignificant for LC-DAD only, and the average preconcentration factor was about 60 times. Recoveries ranged from 94 to 113% for LC-DAD and 95-115% for LC-MS/MS analysis. ANOVA was applied to estimate the standard deviation under repeatability (6.96-8.61% for LC-DAD and 5.98-7.41% for LC-MS/MS) and within-reproducibility (6.96-8.61% for LC-DAD and 6.56-7.41% for LC-MS/MS) conditions. The limits of detection and quantification for LC-MS/MS analysis were 4.29 and 28.74 ng L-1, respectively, while, for LC-DAD, these limits were 14.29 and 95.81 ng L-1, respectively. The results demonstrated that the developed method was suitable for determining MG in water samples, and the large-volume multiphase, multi-sample electroextraction device proved to be a powerful sample preparation technique to obtain high clean-up and large preconcentration levels, which are of paramount importance for environmental applications.