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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 d 5 ) was used as an internal standard. Analyte and the internal standard were extracted from 100 mL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a C 18 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 (r 2 Z0.99) over the concentration range of 0.05-101 ng/mL. Multiple-reaction monitoring mode (MRM) was used for quantification of ion transitions at m/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.
The 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 d 5) was used as an internal standard. Analyte and the internal standard were extracted from 100 mL of human plasma via solid phase extraction technique using Oasis HLB cartridges. The chromatographic separation was achieved on a C 18 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 (r 2 Z0.99) over the concentration range of 0.05-101 ng / mL. Multiple-reaction monitoring mode (MRM) was used for quantification of ion transitions at m / 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 meet the acceptance criteria. A run time of 2.5 min for each sample made it po ssible to analyze more than 300 plasma samples per day. The proposed method was found to be applicable to clinical studies.