RESUMEN
Objective To develop an HPLC method for the determination of mycophenolic acid(MPA), mycophenolic acid glucuronide(MPAG) in plasma.Methods The samples were precipitated with zinc sulphate-methanol solution before injection.Carbamazepine was selected as internal standard,ZORBAX XDB C18 (4.6 mm ×250 mm,5 μm) column was used and the flow rate was 1 mL/min.The mobile phase consisted of methanol-acetonitrile-potassium dihydrogen phosphate buffer solution(gradient elution) .The column temperature was 30℃ and the detective wave length was 254 nm.And then the MPA,MPAG concentration of 32 patients in 7-14 days after renal transplantion were determined.Results The assay was linear within 0.2-50μg/mL for MPA, 2.5-500 μg/mL for MPAG(r>0.999).Absolute recovery rates of MPA,MPAG were more than 80%, the recoveries were between 90%-110%.The intra-day and inter-day RSDs were both lower than 10%.Totally 32 cases of renal transplantion patiens were with mycophenolate mofetil at the dose of 1-1.5 g/d,and MPA in plasma was within the range of 0.32-6.19μg/mL,MPAG in plasma was within the range of 9.52-149.25μg/mL.Conclusion The method is accurate, convenient and rapid, which could be used in the quantitative determination of plasma concentration of MPA,MPAG in renal transplantion patients.
RESUMEN
Objective: To establish a method for determining mycophenolic acid(MPA) and its glucuronide(MPAG) inhuman plasma. Methods: A high performance liquid chromatographic assay with diode array detection was developed, and thedetector wavelength was set at 254nm. The plasma sample purification was limited to protein precipitation with acetonitrile.The sample was separated on Hypersil ODS2 column (200 mm ?4. 6mm, 5?m), the mobile phase consisted of solution A(25% acetonitrile and 75% 0.02 mol/L KH2PO4,pH 3.0)and solution B(70% acetonitrile and 30% 0.02 mol/L K2HPO4,pH6.5)with gradient elution. The flow rate was 1. 0 ml/min. Results: Calibration curves of MPA and MPAG were linear be-tween 1. 0-5. 0 ?g/ml (r=0.994 4,n=6) and (2.5-100) ?g/ml (r= 0.999 5,n=7),respectively. The detection limit of MPAand MPAG were 0. 5?g/ml, and 1.0 ?g/ml, respectively. The mean recoveries of high, medium and low concentrations ofMPA were (95. 75?2.3l)%, (104.10?1.91) % and (98.11?4.24)%, and MPAG were (97.37?1. 43)%, (101.10?5. 41)%and (105. 44?7.59)%. Conclusion: The present study provides a reliable quantitative method for pharmacokineticstudy and monitor of MPA and MPAG.