Human plasma quantification of fludrocortisone using liquid chromatography coupled with atmospheric pressure chemical ionization mass spectrometry after low-dosage administration.

摘要: Abstract Background Fludrocortisone acetate is given at very low dosage (50 μg) to patients suffering from septic shock with controversial clinical results. However, it not clear if absorption effective in these patients. Methods An analytical method based upon liquid chromatography coupled triple quadrupole spectrometry detection atmospheric pressure chemical ionization interface has been developed for the identification and quantification of fludrocortisone, active molecule circulating human plasma. A solid phase extraction plasma was used after addition fludrocortisone-D2 as internal standard. Compounds were separated on a C18 column gradient methanol–formate buffer. The ion transitions monitor analytes m/z 381 → 239 381 → 181 fludrocortisone 383 → 239 383 → 181 fludrocortisone-D2. Results Retention times 4.0 min both compounds. Calibration curves linear 0.1–25 ng/ml range. limits 0.05 ng/ml 0.1 ng/ml, respectively. intra- inter-assay precisions lower than 10.9% recovery 101.8%. slight matrix effect by about 10% observed. Application patient treated one 50-μg dose shown maximal concentration 0.36 ng/ml obtained 2 h. Conclusion This allows pharmacokinetic/pharmacodynamic studies when an intensive care unit case adrenal insufficiency during shock.