A simple, rapid and sensitive liquid chromatography-tandem mass spectrometric （LC MS/ MS） assay method has been developed and fully validated for the simultaneous quantification of atorvastatin, metformin and g.）im...A simple, rapid and sensitive liquid chromatography-tandem mass spectrometric （LC MS/ MS） assay method has been developed and fully validated for the simultaneous quantification of atorvastatin, metformin and g.）imepiride in human plasma. Carbamazepine was used as internal standard （IS）. The analytes were extracted from 200 μL aliquots of human plasma via protein precipitation using acetonitrile, The reconstituted samples were chromatographed on a Alltima HP C18 column by using a 60：40 （v/v） mixture of acetonitrile and 10 mM ammonium acetate （pH 3.0） as the mobile phase at a flow rate of 1.1 mL/min. The calibration curves obtained were linear （r2〉0.99） over the concentration range of 0.50-150.03 ng/mL for atorvastatin, 12.14-1207.50 ng/mL for metformin and 4.98-494.29 ng/mL for glimepiride. The API-4000 LC-MS/MS in multiple reaction monitoring （MRM） mode was used for detection. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. All the analytes were found to be stable in a battery of stability studies. The method is precise and sensitive enough for its intended purpose. A run time of 2.5 rain for each sample made it possible to analyze more than 300 plasma samples per day. The developed assay method was successfully applied to a pharmacokinetic study in human male volunteers.展开更多
This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was us...This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.展开更多
文摘A simple, rapid and sensitive liquid chromatography-tandem mass spectrometric （LC MS/ MS） assay method has been developed and fully validated for the simultaneous quantification of atorvastatin, metformin and g.）imepiride in human plasma. Carbamazepine was used as internal standard （IS）. The analytes were extracted from 200 μL aliquots of human plasma via protein precipitation using acetonitrile, The reconstituted samples were chromatographed on a Alltima HP C18 column by using a 60：40 （v/v） mixture of acetonitrile and 10 mM ammonium acetate （pH 3.0） as the mobile phase at a flow rate of 1.1 mL/min. The calibration curves obtained were linear （r2〉0.99） over the concentration range of 0.50-150.03 ng/mL for atorvastatin, 12.14-1207.50 ng/mL for metformin and 4.98-494.29 ng/mL for glimepiride. The API-4000 LC-MS/MS in multiple reaction monitoring （MRM） mode was used for detection. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. All the analytes were found to be stable in a battery of stability studies. The method is precise and sensitive enough for its intended purpose. A run time of 2.5 rain for each sample made it possible to analyze more than 300 plasma samples per day. The developed assay method was successfully applied to a pharmacokinetic study in human male volunteers.
文摘This paper describes a simple, rapid and sensitive liquid chromatography tandem mass spectrometry assay for the determination of duloxetine in human plasma. A duloxetine stable labeled isotope （duloxetine ds） was used as an internal standard. Analyte and the internal standard were extracted from 100 btL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a Cl8 column by using a mixture of acetonitrile 5 mM ammonium acetate buffer （83：17, v/v） as the mobile phase at a flow rate of 0.9 mL/min. The calibration curve obtained was linear （r2≥0.99） over the concentration range of 0.05 101 ng/mL. Multiple-reaction monitoring mode （MRM） was used for quantification of ion transitions at rn/z 298.3/154.1 and 303.3/159.1 for the drug and the internal standard, respectively. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.
