Sensitive and selective assay for fentanyl using gas chromatography with mass selective detection

摘要: A modified gas chromatographic assay, using mass-selective detection, has been developed for the quantitation of fentanyl in swine serum. Fentanyl and sufentanil, internal standard, were extracted a single-step liquid-liquid extraction with dichloromethane. Sensitivity selectivity improved by electron-impact ionization (EI) selected-ion monitoring (SIM) mode, where sufentanil monitored fragment ions at m/z 245 289, respectively. The limit (LOQ) is 0.05 ng/ml, 1 ml sample, C.V. 10.8% signal-to-noise ratio 29. Standard curves linear (r2 = 0.999) over working range 0.05–1.5 1/y2 as weighting factor. Recoveries averaged 69.8 ± 4.7%, 91.0 13.0% 90.9 10.3% serum concentrations 1.5, 0.5 0.1 Intra- inter-day variances, <12% <10% 0.5, 1.5 ng/ml. Bias was 6.2% LOQ ⩽12.8% every other standard curve concentration. Applicability assay demonstrated pharmacokinetic study transdermally administered postoperative swine.