Water is an essential part of life, however, with continued modernization, it has become a dumping place for many pollutants including dyes. The polluted water can severely affect human health. Polluted water can enter into the human body through different channels, including the food web. Thus, it is very important for human beings and animals to have access to pollution free water. To get the knowledge of the pollutants, in this case, a dye, we need sensitive analytical procedure which could tell the amount of dye in water and also steps to get the pollutant removed from water. In this work, a liquid chromatography–mass spectrometry (LC-MS/MS) based analytical method was developed to determine malachite green. The method was developed after proper optimization of the experimental conditions, where finally, ethanol, a green solvent and formic acid, a food additive was selected to constitute the mobile phase in ratio 1.5:1.0. Different validation parameters were used to authenticate the reliability of the method. Based on the experiment results, the method was found to be linear in the range of 0.1 to 10 mg/L with an excellent correlation coefficient of 0.9995. The corresponding linear regression equation was found to be A = −6863.2 + 105,520 C; where A is the area of the peak and C is the concentration of malachite green. The precision study proves the reproducibility of LC-MS/MS procedure, throughout the precision experiment percent relative standard deviation (% RSD) was found to be between 0.709–1.893%. Similarly, the experiments on the recovery suggest a recovery of 97.28–98.75%. The new method was applied to check the amount of malachite green in environmental samples including the industrial wastewater. The wastewater sample was extracted using the solid phase extraction (SPE) technique, where a new adsorbent—wood apple hydrochar—was synthesized and used as the solid phase for the preparation of a solid phase extraction column to extract the malachite green. The synthesized adsorbent was characterized using different techniques. To conclude, the developed method can be used for determination of malachite green in environmental samples, and the SPE technique using wood apple hydrochar can successfully extract the dye from the water samples.
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