JOURNAL OF CHILEAN CHEMICAL SOCIETY

Vol 63 No 1 (2018): Journal of the Chilean Chemical Society
Original Research Papers

HIGH THROUGHPUT ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY - MASS SPECTROMETRIC METHOD FOR DETERMINATION OF ADRENALINE AND CHARACTERIZATION OF ITS STRESS DEGRADATION PRODUCTS: A MECHANISTIC APPROACH

Masoom R. Siddiqui
Advanced Materials research Chair, Department of chemistry, College of Science, King Saud University, Riyadh
Saikh M. Wabaidur
Advanced Materials research Chair, Department of chemistry, College of Science, King Saud University, Riyadh
Zeid A. Alothman
Advanced Materials research Chair, Department of chemistry, College of Science, King Saud University, Riyadh
M.Z.A. Rafiquee
Department of Applied Chemistry, Aligarh Muslim University, Aligarh
Moonis Ali Khan
Advanced Materials research Chair, Department of chemistry, College of Science, King Saud University, Riyadh
Sadia Sumbul
Department of Chemistry, College of Science, Princess Noura Bint Abdul Rehman University, Riyadh
Published April 25, 2018
Keywords
  • Adrenaline,
  • UPLC-MS method,
  • pharmaceutical analysis,
  • forced degradation study

Abstract

UPLC-MS analytical procedure has been established for the determination of adrenaline in marketed formulation and in the pure form. The detection of the adrenaline was executed considering positive electrospray ionization (ESI) and selected ion reaction (SIR) modes. Chromatographic separation was achieved using ACQUITY UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm particles size) using a binary mobile phase mixture of methanol and water (50:50). The mobile phase was set to flow at the rate of 0.3 ml min-1. The run time time for adrenaline was as short as 1.5 minutes. Linearity was found to be over the concentration range of 1μg ml-1 - 6μg ml-1. An excellent recovery of 100.18 % - 100.68 % was achieved using this procedure. The standard deviation ranged from 0.014 - 0.118 in intra-day studies and 0.016 - 0.096 in case of inter-day studies. The procedure’s quantitation limit was 0.76μg ml-1 and detection limit was 0.25 μg ml-1. The method was successfully applied to determine adrenaline in drug formulations. In order to get the information about the stability of adrenaline in various environments forced degradation studies were conducted and the characterization of the stressed samples were performed using mass spectrometry.

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