DOI: https://doi.org/10.24959/ophcj.19.974

Development and validation of GLC/MS-procedure of doxylamine quantitative determination

L. Yu. Klimenko, S. M. Trut, T. A. Kostina, S. M. Poluyan

Abstract


Doxylamine is a hypnotic medicine used for treatment of minor sleep disorders and is a frequent cause of poisoning.
Aim. To develop GLC/MS-procedure of doxylamine quantification and carry out step-by-step validation of
the developed procedure in the variants of the method of calibration curve, method of standard and method of additions.
Results. The chromatographic conditions have been chosen for doxylamine determination by the method of GLC with mass-spectrometry detection with temperature program changing during the analysis from 70 °C to 320 °C. Retention time for doxylamine is 14.53 min. To prove the possibility of the proposed procedure application in further analysis its validation has been carried out in the variants of the method of calibration curve, method of standard and method of additions. Such validation parameters as in process stability, linearity, accuracy, precision and limit of determination have been estimated by model solutions.
Experimental part. Conditions of chromatographic analysis: Agilent 6890N/5973N/7683; НР-5MS ∅0.25 mm × 30 m, 0.25 μm; DB-17MS ∅0.25 mm × 30 m, 0.15 μm; columns are connected sequentially through Deans switch; thermostat – 70 CºС (2 min), 45 ºС/min to 210 ºС, 6 ºС/min to 320 ºС (12.56 min); transfer line – 280 ºС; ion source – 230 ºС; quadrupole – 150 ºС; electron impact, 70eV; 40 – 750 m/z; injector – 250 ºС; splitless mode; inlet carrier gas (helium) pressure: 1st column – 26.06 psi, 2nd column – 19.30 psi.
Conclusions. New procedure of doxylamine quantitative determination by the method of GLC/MS has been developed. Its validation has been carried out and acceptability for application has been shown.


Keywords


doxylamine; gas-liquid chromatography; validation

References


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