title: Sensitive liquid chromatography tandem mass spectrometry method for the quantification of sitagliptin, a DPP-4 inhibitor, in human plasma using liquid-liquid extraction.
abstract: A sensitive high-performance liquid chromatography-positive ion electrospray tandem mass spectrometry method was developed and validated for the quantification of sitagliptin, a DPP-4 inhibitor, in human plasma. Following liquid-liquid extraction, the analytes were separated using an isocratic mobile phase on a reverse-phase column and analyzed by MS/MS in the multiple reaction monitoring mode using the respective [M + H](+) ions, m/z 408-235 for sitagliptin and m/z 310-148 for the internal standard. The assay exhibited a linear dynamic range of 0.1-250 ng/mL for sitagliptin in human plasma. The lower limit of quantification was 0.1 ng/mL with a relative standard deviation of less than 6%. Acceptable precision and accuracy were obtained for concentrations over the standard curve range. A run time of 2.0 min for each sample made it possible to analyze more than 300 human plasma samples per day. The validated method has been successfully used to analyze human plasma samples for application in pharmacokinetic studies.
authors.affiliation: Biopharmaceutical Research, Suven Life Sciences Ltd, Serene Chambers, Road-5, Avenue-7, Banjara Hills, Hyderabad 500034, India. Ramakrishna_nirogi@yahoo.co.in
authors.forename: Ramakrishna
authors.initials: R
authors.lastname: Nirogi
authors.forename: Vishwottam
authors.initials: V
authors.lastname: Kandikere
authors.forename: Koteshwara
authors.initials: K
authors.lastname: Mudigonda
authors.forename: Prashanth
authors.initials: P
authors.lastname: Komarneni
authors.forename: Raghupathi
authors.initials: R
authors.lastname: Aleti
authors.forename: Rajeshkumar
authors.initials: R
authors.lastname: Boggavarapu
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D018819:Dipeptidyl Peptidase 4; D054873:Dipeptidyl-Peptidase IV Inhibitors; D006801:Humans; D011719:Pyrazines / Q000097:blood* / Q000737:chemistry / Q000302:isolation & purification; D015203:Reproducibility of Results; D000068900:Sitagliptin Phosphate; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D014230:Triazoles / Q000097:blood* / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D054873:Dipeptidyl-Peptidase IV Inhibitors; D011719:Pyrazines; D014230:Triazoles; C042807:DPP4 protein, human; D018819:Dipeptidyl Peptidase 4; D000068900:Sitagliptin Phosphate