Sodium dodecyl sulfate-multi-walled carbon nanotubes-coated-membrane solid phase extraction of glucocorticoids in aqueous matrices

A membrane-based solid phase extraction (SPE)-ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the determination of nine glucocorticoids in water. This new hybrid SPE approach involved the deposition of sodium dodecyl sulfate (SDS)-multi-walled carbon nanotubes (MWCNTs) on a piece of polypropylene membrane that served as the extraction device. Hitherto, such a sample preparation procedure has not been applied to the analysis of water contaminants before. The use of the surfactant helped to disperse the MWCNTs effectively so that they were coated uniformly onto the polypropylene membrane. This increased the overall extraction efficiency of the procedure. Characterisation of the SDS-MWCNTs material was performed using transmission electron microscopy and scanning electron microscopy. The membrane device did not require a pre-conditioning step. The most favourable extraction parameters such as type of surfactant, percentage of surfactant, type of desorption solvent, stirring rate, desorption time, extraction time, temperature, salting-out effect, pH and diameter of MWCNTs were obtained. The method showed linearity ranges from 0.2 to 100 ng mL(-1) for hydrocortisone, dexamethasone, cortisone acetate and beclomethasone dipmpionate, and 0.5-100 ng mL(-1) for the rest of the analytes. Limits of detection ranging from 0.019 to 0.098 ng mL(-1), and limits of quantification ranging from 0.065 to 0.326 ng mL(-1), were obtained for the analytes. The intra-day repeatability was between 1.77 and 3.56% while the inter-day reproducibility was between 2.69 and 9.53%, respectively. The method was used to analyse glucocorticoids as contaminants in the canal water samples.

Automated summary

A novel membrane-based SPE-UHPLC-MS/MS method was developed for the determination of nine glucocorticoids in water, with the use of SDS-MWCNTs material and membrane device, enhancing the overall extraction efficiency.