Rapid screening and determination of fentanyl and its analogues in drugs by liquid chromatography-quadrupole time-of-flight mass spectrometry

A method based on liquid chromatography coupled with high-resolution quadrupole time-of-flight mass spectrometry ( LC. QTOF. MS) was developed for the simultaneous screening and determination of fentanyl and its 26 analogs in liquid and solid powder drugs. The estab. lished method involves successive extraction by 5 mL 75% ( v / v) acetonitrile aqueous solution and 5 mL acetonitrile, followed by clean.up using the hydrophilic lipophilic balance ( HLB) solid. phase extraction method. Detection was achieved by electrospray ionization ( ESI) in the positive mode, TOF. MS, and information. dependent acquisition ( IDA). MS / MS acquisition; the external standard method was adopted for quantification. Two databases of accurate mass and fragment ions were created. The standard matrix. matched calibration curves of the 27 target compounds were linear in the range of 5.. 00- 100 mu g / L, with the correlation coefficients ( r2) >0. 99. The limits of quantification for the 27 target compounds were 10.. 0 mu g / kg. The recover. ies for all the target compounds in vitamin C tablet, headache powder, cough syrup, and trans. dermal patch samples were in the ranges of 82.. 9% - 106%, 84.. 8% - 106%, 86.. 9% - 109%, and 83.. 1% -106%, respectively, with relative standard deviations ranging from 0.. 38% to 8.. 71% ( n = 6). The results demonstrated that the developed method is rapid and sensitive for the simulta. neous monitoring and determination of fentanyl and 26 its analogs in liquid and solid powder drugs.