An electrochemical sensor for ifosfamide, acetaminophen, domperidone, and sumatriptan based on self-assembled MXene/MWCNT/chitosan nanocomposite thin film.

New multi-walled carbon nanotubes supported on Ti3C2-MXene and chitosan (chit) composite film-based electrochemical sensor for ifosfamide (IFO), acetaminophen (ACOP), domperidone (DOM), and sumatriptan (SUM) have been developed. Ti3C2-MXene was synthesized by a fluoride method. Structural and chemical characterizations suggested the successful preparation of Ti3C2-MXene with clearly seen layered morphology, defined 0 0 2 diffraction peak at 7.5° and complete absence of 1 0 4 plane at 39°. The electrochemical performance of the sensor was investigated by cyclic voltammetry and adsorptive stripping differential pulse voltammetry. The Ti3C2/MWCNT/Chit modified glassy carbon electrode exhibits enhanced electrocatalytic activities toward the oxidation of target analytes. Excellent conductivity, large surface area, and high catalytic properties of the Ti3C2-MXene showed synergistic effects with MWCNTs and helped in achieving low detection limits of targets with high selectivity and reproducibility. The assay allows determination of IFO, ACOP, DOM, and SUM in the concentration ranges 0.0011-1.0, 0.0042-7.1, 0.0046-7.3, and 0.0033-61 µM with low detection limits of 0.00031, 0.00028, 0.00034, and 0.00042 µM, respectively. The sensor was successfully applied for voltammetric screening of target analytes in urine and blood serum samples with recoveries > 95.21%. Schematic illustration of the synthesis of self-assembled MXene/MWCNT/chitosan nanocomposite is given and its application to the voltammetric determination of ifosfamide, acetaminophen, domperidone, and sumatriptan described. Graphical abstract.

Validation of a liquid chromatographic tandem mass spectrometric method for the determination of sumatriptan in human biological fluids.

A liquid chromatographic tandem mass spectrometric method for the quantitative determination of sumatriptan base in human plasma and urine has been developed and validated over the concentration range 0.2-20 ng base ml-1. Sumatriptan is a 5-HT1 receptor agonist which has found widespread use in the treatment of migraine. Sumatriptan and its internal standard (D3-sumatriptan) were extracted from human matrices using C2 solid phase cartridges. The extracts were chromatographed on a C18 column, ionised using a heated nebuliser assisted atmospheric pressure ionisation (API) interface and detected by MS/MS in the multiple reaction monitoring mode. The completed validation demonstrated the method to be robust, accurate, precise and specific for the direct quantification of sumatriptan in human fluids. The method was used on a routine basis to determine the levels of sumatriptan in human volunteers following the oral administration of a 25 mg dose of sumatriptan succinate.

Screening and identification of sumatriptan and its main metabolite by means of thin-layer chromatography, ultraviolet spectroscopy and gas chromatography/mass spectrometry.

Sumatriptan (CAS 103628-46-2, 3-[2-(dimethylamino)ethyl]-N-methyl-1H-indole-5-methanesulphonamide++ +), a substance for treatment of acute migraine attacks, and its main metabolite are investigated by thinlayer chromatography (TLC), ultraviolet spectroscopy, and gas chromatography/mass spectrometry (GC/MS). The resulting analytical data (correlated hRf-values, UV solvent spectra, remission spectra, GC retention indices, and electron impact (EI) mass spectra) including an extraction procedure and different derivatization methods are presented. Their applicability is described for urine analysis.