Abstract

A new green method using water as the extraction solvent and golden mussel shell as the solid support in vortex-assisted matrix solid phase dispersion (VA-MSPD) has been developed for the determination of acetylisalicylic acid (ASA) and salicylic acid (SA) in sewage sludge samples by liquid chromatography-tandem mass spectrometry (LC/MS-MS). Higher recoveries were achieved when 0.5 g sample was homogenized with 0.5 g of mussel shell and 10 mL of water was used as the extraction solvent. The performance of the method was evaluated through linearity, recovery, precision (intra-day), method detection and quantification limits (MDL and MQL, respectively) and the matrix effect. The calibration curves prepared in water and in the matrix extract showed a correlation coefficient of 0.99. The MQL value was 100 ng g−1 for both analytes. Recoveries between 68 and 120% were reached with relative standard deviations lower than 20% (n = 9) for the compounds. The matrix effect values were 44 and −55% for SA and ASA, respectively, and these values are similar to those found in this type of matrix. The method was successfully applied to real samples and SA was detected below the MQL.

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