Fentanyl, as one of the most widely used opioid drugs with both therapeutic effects an‎d a high potential for abuse, has attracted significant attention in clinical an‎d toxicological studies. Due to its high potency an‎d potential toxicity, the development of rapid, accurate, an‎d cost-effective methods for the identification an‎d quantification of this compound in biological samples is of particular importance. In the present study, Dispersive Liquid–Liquid Microextraction (DLLME) was selec‎ted as an efficient sample extraction technique an‎d optimized for the extraction of fentanyl from biological matrices. For detection, Ion Mobility Spectrometry (IMS) was employed, which, owing to its simplicity, high speed, an‎d adequate separation capability, represents a suitable approach for this class of compounds. During the optimization process, various parameters were investigated, including the type an‎d volume of the extraction solvent (chloroform, chlorobenzene, carbon tetrachloride, an‎d carbon disulfide), the type an‎d volume of the dispersive solvent (methanol, acetone, an‎d acetonitrile), solution pH, centrifugation speed, an‎d centrifugation time. The results indicated that using chloroform as the extraction solvent an‎d methanol as the dispersive solvent provided the highest extraction efficiency. Optimization of volumes revealed that 100 µL of chloroform an‎d 500 µL of methanol constituted the ideal conditions for achieving maximum extraction performance. Furthermore, a pH of 10, a centrifugation speed of 4000 rpm, an‎d a centrifugation time of 7 minutes were selec‎ted as the optimal conditions. eva‎luation of analytical parameters demonstrated a limit of detection of 70 µg L⁻¹, a linear range of 200–8000 µg L⁻¹, relative stan‎dard deviations of 5% within a day an‎d 9.5% over three consecutive days, as well as relative recoveries of 89–112% for fentanyl spiked into real plasma matrices. Assessment of these parameters confirmed that the DLLME–IMS method possesses adequate sensitivity an‎d precision for the measurement of fentanyl at relatively low concentrations. The recoveries were generally within acceptable ranges. Application of the method to real biological samples also provided satisfactory results. Overall, the findings of this study indicate that DLLME in combination with IMS can serve as a rapid, simple, an‎d cost-effective approach for monitoring fentanyl in biological samples. This method reduces the consumption of organic solvents an‎d preparation time, an‎d it is applicable in both clinical studies an‎d forensic toxicology.

محمد تقي جعفري

محمد سراجي , اسماعيل حيدري بفرويي