Highly sensitive assay for the determination of therapeutic peptide desmopressin in human plasma by UPLC-MS/MS.

Journal: Journal of pharmaceutical analysis
Published Date:

Abstract

An analytical method based on ultra-performance liquid chromatography with positive ion electrospray ionization (ESI) coupled with tandem mass spectrometry detection (UPLC-MS/MS) was developed and validated for the determination of therapeutic peptide desmopressin in human plasma. A desmopressin stable labeled isotope (desmopressin d) was used as an internal standard. Analyte and the internal standard were extracted from 200 µL of human plasma solid-phase extraction technique using Oasis WCX cartridges. The chromatographic separation was achieved on an Aquity UPLC HSS T3 column by using a gradient mixture of methanol and 1 mM ammonium formate buffer as the mobile phase. The calibration curve obtained was linear ( ≥0.99) over the concentration range of 1.01-200 pg/mL. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. The results of the intra- and inter-day precision and accuracy studies were well within the acceptable limits. The proposed method was successfully applied to pharmacokinetic studies in humans.

Authors

  • Shiva Kumar Gudlawar
    Department of Chemistry, Banasthali Vidyapeeth, Jaipur 304022, India.
  • Nageswara Rao Pilli
    Wellquest Clinical Research Laboratories, Ramanthapur, Hyderabad 500013, India.
  • Sridhar Siddiraju
    Department of Pharmaceutical Chemistry, Malla Reddy College of Pharmacy, Maisammaguda, Secunderabad 5000100, India.
  • Jaya Dwivedi
    Department of Chemistry, Banasthali Vidyapeeth, Jaipur 304022, India.

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