A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple...A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple protein precipitation of MPA along with its deuterated analog as an internal standard （IS） from 50 mL of human plasma. The chromatographic analysis was done on Acquity UPLC C18 （100mm×2.1mm,1.7μm） column under isocratic conditions using acetonitrile and 10 mM ammonium formate, pH 3.00 （75：25, v/v） as the mobile phase. A triple quadrupole mass spectrometer operating in the positive ionization mode was used for quantitation. In-source conversion of mycophenolic glucuronide metabolite to the parent drug was selectively controlled by suitable optimization of cone voltage, cone gas flow and desolvation temperature. The method was validated over a wide concentration range of 15-15000 ng/mL. The mean extraction recovery for the analyte and IS was 〉95%. Matrix effect expressed as matrix factors ranged from 0.97 to 1.02. The method was successfully applied to support a bioequivalence study of 500 mg mycophenolate mofetil tablet in 72 healthy subjects.展开更多
This paper describes a selective and sensitive assay for the determination of olanzapine(OLZ)in human plasma based on liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analyte and quetiapine as internal sta...This paper describes a selective and sensitive assay for the determination of olanzapine(OLZ)in human plasma based on liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analyte and quetiapine as internal standard(IS)were extracted from 200μL plasma via solid phase extraction on Waters Oasis HLB cartridges.Chromatographic separation was achieved on an ACE 5C18-300 column(100 mm × 4.6 mm,5μm)under isocratic conditions in a run time of 3.5 min.Mass spectrometric detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring(MRM)of the transitions at m/z 313/256 for OLZ and m/z 384/253 for the IS.The assay was linear in the range 0.10-40.0 ng/mL with a lower limit of quantitation and limit of detection of 0.10 and 0.012 ng/mL,respectively.Intra-and inter-day precision(as coefficient of variation)and relative recovery were<5.0% and>90%,respectively.The method was succesfully applied to a bioequivalence study of 5 and 10 mg OLZ disintegrating tablets in 40 healthy Indian males with reproducibility by incurred sample reanalysis in the range-7.43 to 8.07%.展开更多
文摘A simple, sensitive and high throughput ultra performance liquid chromatography tandem mass spectrometry method has been developed for the determination of mycophenolic acid in human plasma. The method involved simple protein precipitation of MPA along with its deuterated analog as an internal standard （IS） from 50 mL of human plasma. The chromatographic analysis was done on Acquity UPLC C18 （100mm×2.1mm,1.7μm） column under isocratic conditions using acetonitrile and 10 mM ammonium formate, pH 3.00 （75：25, v/v） as the mobile phase. A triple quadrupole mass spectrometer operating in the positive ionization mode was used for quantitation. In-source conversion of mycophenolic glucuronide metabolite to the parent drug was selectively controlled by suitable optimization of cone voltage, cone gas flow and desolvation temperature. The method was validated over a wide concentration range of 15-15000 ng/mL. The mean extraction recovery for the analyte and IS was 〉95%. Matrix effect expressed as matrix factors ranged from 0.97 to 1.02. The method was successfully applied to support a bioequivalence study of 500 mg mycophenolate mofetil tablet in 72 healthy subjects.
文摘This paper describes a selective and sensitive assay for the determination of olanzapine(OLZ)in human plasma based on liquid chromatography-tandem mass spectrometry(LC-MS/MS).The analyte and quetiapine as internal standard(IS)were extracted from 200μL plasma via solid phase extraction on Waters Oasis HLB cartridges.Chromatographic separation was achieved on an ACE 5C18-300 column(100 mm × 4.6 mm,5μm)under isocratic conditions in a run time of 3.5 min.Mass spectrometric detection involved electrospray ionization in the positive ion mode followed by multiple reaction monitoring(MRM)of the transitions at m/z 313/256 for OLZ and m/z 384/253 for the IS.The assay was linear in the range 0.10-40.0 ng/mL with a lower limit of quantitation and limit of detection of 0.10 and 0.012 ng/mL,respectively.Intra-and inter-day precision(as coefficient of variation)and relative recovery were<5.0% and>90%,respectively.The method was succesfully applied to a bioequivalence study of 5 and 10 mg OLZ disintegrating tablets in 40 healthy Indian males with reproducibility by incurred sample reanalysis in the range-7.43 to 8.07%.
