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Development and validation of a green dispersive liquid-liquid microextraction-LC-MS/MS method for sotalol
Ahmed Serag1, Maram H Abduljabbar2, Manal E Alosaimi3
1Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Al- Azhar University, Nasr City, Cairo, 11751, Egypt. ahmedserag777@hotmail.com.
None:
An LC-MS/MS method coupled with central composite design (CCD)-optimized dispersive liquid-liquid microextraction (DLLME) was developed and validated for sotalol quantification in human plasma according to ICH M10 guidelines. CCD with response surface methodology systematically evaluated four DLLME parameters - disperser solvent volume, extraction solvent volume, sample pH, and centrifugation time - identifying extraction solvent volume, pH, and disperser volume as dominant factors governing extraction efficiency. Optimal conditions of disperser volume 1200 µL, extraction solvent 300 µL, pH 10.0, and centrifugation time 3 min yielded predicted recovery of 95.29%, experimentally confirmed at 99-103%, with organic solvent consumption of 1.5 mL per sample representing a reduction compared to conventional SPE and LLE approaches. Chromatographic separation was achieved on a Poroshell 120 EC-C18 column (100 × 2.1 mm, 2.7 μm) with 4-min isocratic elution, and quantification employed MRM transitions m/z 273.1→255.1 for sotalol and m/z 267.2→145.1 for atenolol internal standard in positive ESI mode. The method demonstrated excellent linearity (1-1200 ng/mL, r² = 0.9994), sensitivity (LLOQ 1 ng/mL), acceptable accuracy and precision, and comprehensive stability under multiple storage conditions, in full compliance with ICH M10 acceptance criteria. Preliminary pharmacokinetic application in healthy volunteers following single oral 80 mg sotalol administration yielded Cmax 701 ± 53.8 ng/mL, t½ 10.1 ± 1.0 h, and AUC0→∞ 11,713 ± 1,345 ng·h/mL, broadly consistent with published literature values, supporting method applicability for therapeutic drug monitoring. Multi-metric sustainability assessment encompassing AGSA-prep (64/100), AGSA (65.28/100), CaFRI (69/100), BAGI (75.0/100), CACI (69/100), AMRI (71/100), and WECA (81%) demonstrated improved environmental performance relative to conventional extraction approaches, providing comprehensive sustainability characterization of the developed method.
